CN116179198B - Method for preparing solid rare earth doped fluorescent carbon dots by one-step hydrothermal method - Google Patents
Method for preparing solid rare earth doped fluorescent carbon dots by one-step hydrothermal method Download PDFInfo
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 59
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 55
- 239000007787 solid Substances 0.000 title claims abstract description 41
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000001027 hydrothermal synthesis Methods 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 15
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 18
- XFNJVKMNNVCYEK-UHFFFAOYSA-N 1-naphthaleneacetamide Chemical compound C1=CC=C2C(CC(=O)N)=CC=CC2=C1 XFNJVKMNNVCYEK-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910003451 terbium oxide Inorganic materials 0.000 claims abstract description 15
- SCRZPWWVSXWCMC-UHFFFAOYSA-N terbium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Tb+3].[Tb+3] SCRZPWWVSXWCMC-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002244 precipitate Substances 0.000 claims abstract description 12
- 239000007864 aqueous solution Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 238000000746 purification Methods 0.000 claims abstract description 8
- 239000000047 product Substances 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 11
- FWFGVMYFCODZRD-UHFFFAOYSA-N oxidanium;hydrogen sulfate Chemical compound O.OS(O)(=O)=O FWFGVMYFCODZRD-UHFFFAOYSA-N 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims 2
- 238000004090 dissolution Methods 0.000 claims 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 25
- 229910052799 carbon Inorganic materials 0.000 abstract description 25
- 238000002360 preparation method Methods 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 6
- 230000005284 excitation Effects 0.000 abstract description 4
- 238000004020 luminiscence type Methods 0.000 abstract description 4
- 238000010791 quenching Methods 0.000 abstract description 2
- 230000000171 quenching effect Effects 0.000 abstract description 2
- 229910052771 Terbium Inorganic materials 0.000 abstract 1
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 239000008367 deionised water Substances 0.000 description 9
- 229910021641 deionized water Inorganic materials 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 5
- -1 rare earth compound Chemical class 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000000862 absorption spectrum Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000002189 fluorescence spectrum Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 230000001419 dependent effect Effects 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 description 2
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 2
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000695 excitation spectrum Methods 0.000 description 1
- 238000002284 excitation--emission spectrum Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 238000011403 purification operation Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
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- 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
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7743—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing terbium
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- 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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- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
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Abstract
The invention provides a method for preparing solid rare earth doped fluorescent carbon dots by a one-step hydrothermal method. The method comprises the following steps: firstly, dissolving naphthalene acetamide and terbium oxide in sulfuric acid aqueous solution, fully stirring, then carrying out hydrothermal reaction in a reaction kettle, and taking out after cooling to room temperature to obtain a primary product; and (3) performing centrifugal purification on the obtained initial product for a plurality of times, and drying the solid precipitate after centrifugal purification to obtain the solid rare earth doped carbon dot material with stable luminescence, wherein the characteristic emission peak of the rare earth terbium can be seen under the excitation of ultraviolet wavelength. The invention belongs to the field of luminescent material preparation, and the carbon dot product prepared by the method disclosed by the invention exists in a solid state, does not have solid state fluorescence quenching, and is stable in luminescence, and the fluorescent performance of the original material is improved by rare earth doping.
Description
Technical Field
The invention relates to the technical field of preparation of carbon quantum dots, in particular to a method for preparing solid rare earth doped fluorescent carbon dots by a one-step hydrothermal method.
Background
The carbon dots are novel nano materials with carbon as a framework structure, and the surface of the novel nano materials has rich functional groups, so that convenience is provided for further compounding. The doping of the carbon dots can change the electron chemical structure of the carbon dots by regulating the energy band gap and the charge density, so as to improve the optical performance of the carbon dots. The application of carbon dots in analytical detection and biomedicine is widened by doping. The doping of the carbon dots mainly comprises nonmetallic doping, transition metal doping and rare earth doping. The luminescent rare earth complex has the advantages of narrow fluorescence peak, good monochromaticity, high fluorescence efficiency and the like. By means of doping, the luminous advantages of carbon dots and rare earth can be maintained, and the weaknesses of the luminous performance of the carbon dots and the rare earth can be made up. However, rare earth metals have high toxicity, and the existing rare earth doping is mainly based on material compounding, so that the preparation steps are complicated. The composite material is mostly used for detection by utilizing the emission peak of a carbon point, but reports on red area emission signals of rare earth metals are less, and the application of the composite material in the analysis sensing field is to be expanded.
Disclosure of Invention
The invention aims to provide a method for preparing solid rare earth doped fluorescent carbon dots by a one-step hydrothermal method, which aims to overcome the defects of the existing rare earth composite material doped carbon dot preparation technology and avoid complex purification steps.
The invention is realized in the following way:
the preparation method of the solid rare earth doped fluorescent carbon dots by a one-step hydrothermal method comprises the following steps: dissolving a carbon source in a sulfuric acid aqueous solution, adding rare earth oxide for full reaction, reacting for 4 hours at 200 ℃, centrifuging, drying and the like to obtain the rare earth doped solid carbon dots.
The carbon source is naphthalene acetamide; the rare earth oxide is terbium oxide. The mass ratio of terbium oxide to naphthalene acetamide is 4:3-2:1.
And (3) centrifugally purifying a solid product containing the rare earth doped carbon dots by deionized water.
The XPS full spectrum and the high-resolution electron spectrum of Tb are obtained through XPS spectrum detection, and the existence of Tb peak can be obviously seen.
The research of the invention finds that:
the preparation method for synthesizing the solid rare earth doped carbon point by using naphthalene acetamide as a carbon source and terbium oxide as a rare earth doped compound through a hydrothermal method in one step specifically comprises the following steps:
(1) Dissolving naphthalene acetamide in sulfuric acid water solution, adding rare earth compound and stirring until completely dissolving;
(2) Placing the uniformly stirred mixed solution into a reaction kettle, and placing the reaction kettle into a drying box for heating;
(3) Taking out after cooling to room temperature, and performing centrifugal purification by using deionized water;
(4) The precipitate obtained after centrifugation and purification was dried.
In the step (1), the mass of the naphthalene acetamide is 0.6g, the rare earth compound is terbium oxide, the mass of the naphthalene acetamide is 0.8-1.2g, and the stirring time is 30-60 min.
The reaction temperature in the step (2) is 200 ℃ and the reaction time is 4 hours.
In the step (3), the rotation speed of the centrifugal machine is 8000rpm, the centrifugal time is 5min, and the centrifugal purification operation is repeated for 2-5 times.
In the step (4), the temperature of the drying box is set to 80 ℃ and the time is set to 4 hours.
The invention has the beneficial effects that:
(1) According to the invention, naphthalene acetamide is used as a single carbon source, terbium oxide is used as a doping material, and a solid rare earth doped carbon point is obtained. The method is simple in preparation, the selected rare earth compound can be subjected to experiments without further treatment, and the prepared carbon dots exist in a solid state, so that the luminous performance of the rare earth and the carbon dots is maintained.
(2) The solid rare earth doped carbon point can be subjected to subsequent testing after centrifugation and drying without complex purification steps.
(3) The carbon dot product prepared by the method disclosed by the invention exists in a solid state, solid state fluorescence quenching does not exist, luminescence is stable, and the fluorescence performance of the original material is improved by rare earth doping.
Drawings
FIG. 1 is a spectrum of an X-ray spectrometer of a solid rare earth doped carbon dot prepared in example 1 of the present invention.
FIG. 2 shows Tb of a solid rare earth doped carbon dot prepared in example 1 of the present invention 3+ Is a high resolution electron energy spectrum of (c).
FIG. 3 is an infrared absorption spectrum of a solid rare earth doped carbon dot prepared in example 1 of the present invention.
FIG. 4 is a fluorescence excitation spectrum of a solid rare earth doped carbon dot prepared in example 1 of the present invention.
Fig. 5 shows emission spectra of solid rare earth doped carbon dots prepared in example 1 of the present invention at different excitation wavelengths.
FIG. 6 is an ultraviolet-visible absorption spectrum of a solid rare earth doped carbon dot prepared in example 1 of the present invention.
FIG. 7 shows the effect of different doping ratios on solid rare earth doped carbon dots according to examples 1-3 of the present invention.
FIG. 8 is a fluorescence spectrum of the carbon dots prepared in comparative example 1.
Detailed Description
Example 1
The method for preparing the solid fluorescent carbon dots by utilizing the naphthalene acetamide and terbium oxide through a one-step hydrothermal method specifically comprises the following steps:
(1) Dissolving 0.6g of naphthalene acetamide in 10mL of sulfuric acid water solution, stirring for 0.5h until the solution is transparent and colorless, then adding 0.8g of terbium oxide into the solution, stirring for 0.5h, and fully reacting; wherein, the sulfuric acid aqueous solution is prepared from 98% concentrated sulfuric acid and deionized water according to the volume ratio of 1: 1.
(2) The mixed solution is placed in a reaction kettle for hydrothermal reaction, magnetic stirring is carried out for 30min, and the reaction kettle is placed in a drying oven at 200 ℃ for heating for 4h.
(3) And after the reaction is finished, taking the precipitate, using deionized water as an extracting agent, putting the precipitate into a centrifugal machine, centrifuging for 5min at the rotating speed of 8000rpm, and repeating the centrifugal operation four times to ensure that impurities are removed.
(4) And (3) placing the centrifuged solid precipitate in a drying box at 80 ℃ for drying for 4 hours to obtain pure rare earth Tb doped carbon dots (Tb-CDs/0.8).
The XPS element analysis data of the solid powder is measured by taking a proper amount of rare earth Tb doped carbon points, and as shown in fig. 1 and 2, the prepared solid rare earth doped fluorescent carbon points are successfully doped with Tb.
Mixing carbon dot powder with potassium bromide, tabletting with a tablet press, and performing infrared absorption spectrum test, excitation emission and fluorescence spectrum test under different excitation light to obtain the results shown in figures 3-5. As can be seen from fig. 3, the solid rare earth doped fluorescent carbon dots contain abundant N, O functional groups, and Tb-O bonds are present in the fingerprint region. As can be seen from fig. 5, the solid rare earth doped fluorescent carbon dots maintain the luminescent characteristics of the carbon dots and rare earth.
1g of rare earth Tb doped carbon dot powder is dispersed into 30mL of deionized water, and uniformly stirred to obtain rare earth Tb doped carbon dot aqueous solution, and the ultraviolet-visible spectrum under the state of the solution is measured, and the obtained result is shown in figure 6.
Example 2
The procedure for preparing the solid rare earth doped fluorescent carbon dots was the same as in example 1, except that the mass of terbium oxide was 1.0g:
(1) 0.6g of naphthalene acetamide is dissolved in sulfuric acid aqueous solution, and then 0.8g of terbium oxide is added for full reaction, wherein the sulfuric acid aqueous solution is prepared from 98% concentrated sulfuric acid and deionized water according to a volume ratio of 1: 1.
(2) Stirring on a magnetic stirrer for 30min, and heating in a drying oven at 200deg.C for 4 hr.
(3) And after the reaction is finished, taking the precipitate, using deionized water as an extracting agent, putting the precipitate into a centrifugal machine, centrifuging for 5min at the rotating speed of 8000rpm, and repeating the centrifugal operation four times to ensure that impurities are removed.
(4) And (3) placing the centrifuged solid precipitate in a drying box at 80 ℃ for drying for 4 hours to obtain pure rare earth Tb doped carbon dots (Tb-CDs/1.0).
Example 3
The procedure for preparing the solid rare earth doped fluorescent carbon dots was the same as in example 1, except that the mass of terbium oxide was 1.2g:
(1) 0.6g of naphthalene acetamide is dissolved in sulfuric acid aqueous solution, and then 1.2g of terbium oxide is added for full reaction, wherein the sulfuric acid aqueous solution is prepared from 98% concentrated sulfuric acid and deionized water according to a volume ratio of 1: 1.
(2) Stirring on a magnetic stirrer for 30min, and heating in a drying oven at 200deg.C for 4 hr.
(3) And after the reaction is finished, taking the precipitate, using deionized water as an extracting agent, putting the precipitate into a centrifugal machine, centrifuging for 5min at the rotating speed of 8000rpm, and repeating the centrifugal operation four times to ensure that impurities are removed.
(4) And (3) placing the centrifuged solid precipitate in a drying box at 80 ℃ for drying for 4 hours to obtain pure rare earth Tb doped carbon dots (Tb-CDs/1.2).
The solid rare earth doped fluorescent carbon dots prepared in examples 1-3 were excited with 360nm laser, respectively, and the results are shown in FIG. 7. As can be seen from fig. 7, the solid rare earth doped fluorescent carbon dots have concentration-dependent characteristics, and the rare earth luminescence is gradually enhanced as the rare earth compound increases.
Comparative example 1
Dissolving 0.6g of naphthalene acetamide in sulfuric acid water solution, transferring to a polytetrafluoroethylene reaction kettle, capping and sealing, then placing into a drying oven for heating reaction at 200 ℃, reacting for 4 hours, cooling to room temperature, and removing to obtain the solution, namely the carbon dot water solution without doping rare earth.
Fluorescence spectrum test is carried out on the prepared undoped rare earth carbon dot aqueous solution, and the obtained result is shown in fig. 8. As can be seen from fig. 8, the carbon dots without rare earth doping have excitation-dependent characteristics.
Claims (3)
1. A method for preparing solid rare earth doped fluorescent carbon dots by a one-step hydrothermal method is characterized by comprising the following steps:
a. preparing rare earth doped carbon dots by a hydrothermal method: dissolving naphthalene acetamide and terbium oxide in sulfuric acid water solution, fully stirring, then carrying out hydrothermal reaction in a reaction kettle, cooling to room temperature after the reaction is finished, and then taking out to obtain an initial product;
b. c, performing centrifugal purification on the initial product obtained in the step a for a plurality of times, and drying the solid precipitate after centrifugal purification to obtain solid rare earth doped fluorescent carbon dots;
in the step a, the mass ratio of terbium oxide to naphthalene acetamide is 4:3-2:1; the temperature of the hydrothermal reaction was set to 200℃and the reaction time was 4h.
2. The method for preparing solid rare earth doped fluorescent carbon dots by a one-step hydrothermal method according to claim 1, wherein the step a is specifically: weighing 0.6g naphthalene acetamide, adding into 10mL sulfuric acid aqueous solution for dissolution, stirring 0.5h until the solution is transparent and colorless, weighing 0.8-1.2g terbium oxide, dissolving in the solution, stirring 0.5h for full reaction; and (3) placing the mixed solution into a reaction kettle for hydrothermal reaction, and taking out after cooling to room temperature.
3. The method for preparing solid rare earth doped fluorescent carbon dots by a one-step hydrothermal method according to claim 1, wherein in the step b, centrifugation is performed for 5min at 8000rpm for 2-5 times, the drying temperature is 80 ℃, and the drying time period is set to be 4h.
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- 2023-02-27 CN CN202310172511.0A patent/CN116179198B/en active Active
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