CN112920799A - Method for preparing rare earth doped yttrium oxide fluorescent nanoparticles by DBD technology - Google Patents
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Abstract
The invention discloses a method for preparing rare earth doped yttrium oxide fluorescent nanoparticles by a DBD (double-wall double-diffusion) technology, which comprises the following steps: (1) mixing the base metal organic matter and the doped metal organic matter according to the mass ratio of 10-40: 1, and grinding the mixture to be used as a reaction precursor; (2) placing the precursor obtained in the step (1) in a container, wherein the container is placed between a positive electrode and a negative electrode of a plasma reactor; (3) and then, applying alternating current between the cathode and the anode of the plasma reactor in an oxygen atmosphere, treating the precursor for a period of time, taking out products at intervals, and grinding to obtain the powder containing the rare earth doped yttrium oxide nanoparticles. According to the invention, the powder of the rare earth doped yttrium oxide fluorescent nano-particles is prepared by a DBD technology and one-step method by using high-activity oxidation components. The method is simple and easy to implement, green and efficient, does not need high-temperature and high-pressure further reaction, and effectively reduces the energy consumption.
Description
Technical Field
The invention relates to the field of plasma, in particular to a method for preparing rare earth doped yttrium oxide fluorescent nanoparticles by a DBD (double-walled diffusion) technology.
Background
The special electronic configuration of the rare earth elements enables the rare earth elements to have unique optical, electric and magnetic properties, and the rare earth elements are considered as treasures of new materials and vitamins promoting the upgrading of the traditional industry. In recent years, with the development of nanotechnology and life continuity, rare earth nanomaterials integrate rare earth characteristics and nanometer advantages and show multiple peculiar properties such as small-size effect, quantum effect, fluorescence characteristics, photoluminescence and the like. Because the rare earth elements have rich energy levels, the material can emit electric radiation with various wavelengths from infrared light, visible light to ultraviolet light regions by doping different rare earth elements, and because of extremely high imaging sensitivity, high luminous life, low cytotoxicity and excellent light stability, the rare earth doped luminous nano material has huge potential application in clinical medicine.
The synthesis methods of rare earth doped nano materials are various, and mainly comprise a high-temperature solid phase method and a wet chemical method. Although the methods are widely applied, the methods still have some defects.
Patent CN102274969A discloses a method for preparing a rare earth oxide doped molybdenum alloy by using a high-temperature solid phase method, wherein a precursor of the method needs to be subjected to steps of screening, press forming, sintering, forging and vacuum annealing to prepare a target product, and each step needs large energy consumption, has strict requirements on equipment and causes high preparation cost.
Patent CN107217171A discloses a method for doping rare earth composite material with liquid, which inevitably contains raw material impurities during synthesis, and the synthesis process needs to be performed with the steps of evaporative crystallization, drying, baking, doping, reduction, etc., the process is tedious, the consumed time is long, and the product purity is limited due to the existence of impurities, so that the method is difficult to be applied to clinical medicine experimental research.
The preparation of the high-performance luminescent material has extremely high reference value in the field of life science, but the controllability of a high-temperature solid phase method is poor, and the product is not uniform; the wet chemical method generally consumes a long time, the process is complicated, toxic chemical substances such as organic solvents, stabilizers and the like are often involved in the synthesis process, certain harm is caused to human bodies and the environment, and the two methods are difficult to accurately and directly construct related nanostructures on the surface of a specified substrate.
Disclosure of Invention
In view of the above problems in the prior art, the present applicant provides a method for preparing rare earth doped yttrium oxide fluorescent nanoparticles by a DBD technique. According to the invention, the rare earth doped yttrium oxide fluorescent nano powder is prepared by a DBD technology and one-step method by using high-activity oxidation components. The method can be carried out at normal pressure and low temperature, is green and efficient, and has strong controllability on the rare earth doped luminescent nano material.
The technical scheme of the invention is as follows:
a method for preparing rare earth doped yttrium oxide fluorescent nanoparticles by a DBD technique, the method comprising the steps of:
(1) mixing the base metal organic matter and the doped metal organic matter according to the mass ratio of 10-40: 1, and grinding the mixture to be used as a reaction precursor;
(2) placing the precursor obtained in the step (1) in a container, wherein the container is placed between a positive electrode and a negative electrode of a plasma reactor;
(3) and then, applying alternating current between the cathode and the anode of the plasma reactor in an oxygen atmosphere, treating the precursor for a period of time, taking out products at intervals, and grinding to obtain the powder containing the rare earth doped yttrium oxide nanoparticles.
In the step (1), the agglomerated particles in the base metal organic matter and the doped metal organic matter are ground until the particle diameter is less than 0.2 mm.
In the step (1), the base metal organic matter is one or a combination of more than two of yttrium acetylacetonate, molybdenum cyclopentadienyl, yttrium hexafluoroacetylacetonate, molybdenum hexafluoroacetylacetonate, yttrium tris (2,2,6, 6-tetramethyl-3, 5-heptanedionate) and molybdenum tris (2,2,6, 6-tetramethyl-3, 5-heptanedionate).
In the step (1), the doped metal organic matter is europium acetylacetonate, terbium acetylacetonate, dysprosium acetylacetonate, thulium acetylacetonate, cerium acetylacetonate, praseodymium acetylacetonate, samarium acetylacetonate, europium trisulfonate, terbium trisulfonate, dysprosium trisulfonate, thulium trisulfonate, cerium trisulfonate, praseodymium trisulfonate, europium hexafluoroacetylacetonate, terbium hexafluoroacetylacetonate, dysprosium hexafluoroacetylacetonate, thulium hexafluoroacetylacetonate, cerium hexafluoroacetylacetonate, praseodymium hexafluoroacetylacetonate, samarium hexafluoroacetylacetonate, europium tris (2,2,6, 6-tetramethyl-3, 5-heptanedionate), terbium tris (2,2,6, 6-tetramethyl-3, 5-heptanedionate), dysprosium tris (2,2,6, 6-tetramethyl-3, 5-heptanedionate), thulium tris (2, 6, 6-tetramethyl-3, 5-heptanedionate), thulium, One or a combination of two or more of tris (2,2,6, 6-tetramethyl-3, 5-heptanedionate) cerium, tris (2,2,6, 6-tetramethyl-3, 5-heptanedionate) praseodymium and tris (2,2,6, 6-tetramethyl-3, 5-heptanedionate) samarium.
In the step (2), a reaction precursor is placed in a quartz container, and reaction precursor powder is paved at a position 2-3cm away from the center of the container; the top of the container is covered by a quartz plate with a size corresponding to the container.
In the step (2), the diameter of a stainless steel cathode cylinder of the plasma reactor is 50-70 mm, and the height of the stainless steel cathode cylinder is 15-30 mm; the anode and the cathode are the same in size; the distance between the cathode and the anode of the plasma reactor is 10-15 mm.
And (3) regulating and controlling 60-80 sccm of oxygen to be introduced into the container through a mass flow controller, and maintaining until the reaction is completely finished to ensure that the oxygen atmosphere exists all the time in the reaction process.
In the step (3), the applied alternating current ensures that the output power is 100-300W, so as to generate plasma between the positive electrode and the negative electrode.
In the step (3), the time for processing the precursor is 5-30 min.
In the step (3), the product covering the surface of the precursor is collected once every ten minutes, and the product is fully ground to be nano-sized, wherein the particle size is 20-100 nm.
The beneficial technical effects of the invention are as follows:
the invention utilizes the advantages of high DBD technical activity, fast reaction, no pollution, uniform and stable discharge and the like to realize the environment-friendly, fast and controllable preparation of the rare earth doped luminescent nano material at normal pressure and low temperature, and provides a new visual angle for the green controllable preparation of the biomedical nano material.
The reaction can be completed in microsecond level, so that the structural performance of the product can be regulated and controlled.
The reactor disclosed by the invention is simple in structure, convenient to disassemble, high in flexibility, small in occupied area, low in reaction energy consumption, cost-saving and free of a complex post-treatment process. In the reaction process, the reaction atmosphere can be changed by adjusting the gas at the gas inlet, the reaction site can be changed at any time according to the requirements of reactants, and the method is simple, flexible, efficient, safe and cost-saving in operation.
The invention adopts the quartz transparent container, can detect the spectral change in time through an optical fiber spectrometer (optical emission spectrometer) in the reaction process, observe the reaction progress at any time, can adjust the reaction in time, has higher container air tightness, ensures the gas purity in the reaction process, reduces the possibility of generating byproducts and ensures the single product.
Drawings
FIG. 1 is a diagram of an experimental apparatus of the present invention.
FIG. 2 is a TEM morphology of yttrium oxide nanoparticles prepared in example 1 of the present invention;
FIG. 3 is an SEM image of the yttrium oxide nanoparticles prepared in example 1 of the present invention;
FIG. 4 is an EDX spectrum of yttrium oxide nanoparticles prepared in example 1 of the present invention;
FIG. 5 is an XRD pattern of yttrium oxide nanoparticles prepared in example 1 of the present invention.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings and examples.
Example 1
A method for preparing yttrium oxide rare earth doping by DBD technology, the method comprising the steps of:
(1) mixing 0.5g of yttrium acetylacetonate and 0.025g of europium acetylacetonate, and grinding the mixture to obtain a reaction precursor;
(2) placing the precursor obtained in the step (1) in a quartz container, and paving the powder at a position 2.5cm away from the center of the container; the top of the container is covered by a quartz plate with the diameter of 90mm and the thickness of 3 mm; the container is placed between the cathode and the anode of the plasma reactor (the diameter of the electrode cylinder is 56.1mm, the height is 20mm), and the distance between the anode and the cathode is 13 mm;
(3) oxygen of 60sccm is regulated and controlled by a mass flow controller to be introduced into the quartz container, the reaction is maintained until the reaction is completely finished, the existence of oxygen atmosphere is ensured in the reaction process, and the applied alternating current ensures that the output power is 160W, so that plasma is generated between the anode and the cathode. Treating the precursor for 30min, collecting the powder covered on the surface once every ten minutes, and fully grinding the powder until the particle size is 20-100 nm;
the rare earth doping type is changed, the reaction precursor is expanded, a series of rare earth doped luminescent nano materials can be obtained, the number of doping elements can be changed, and the doping of single element is adjusted to be a multi-element co-doping material.
The morphology and elemental characterization of the yttria nanoparticles in the powder prepared in this example are shown in fig. 2-4, and it can be seen from the transmission electron microscope image of fig. 2 that the obtained yttria is formed by the aggregation of irregularly shaped nanoparticles, while the scanning electron microscope image of fig. 3 that the yttria is formed by a loose rod-like structure. In addition, only a few C peaks from air and the rest all yttrium and oxygen peaks in the X-ray spectrum of fig. 4 demonstrate high product purity. The XRD peak positions of fig. 5 are consistent with the standard card of yttria, demonstrating that the purity of yttria in the product is high without other impurity peaks.
Example 2
The preparation method is the same as that of example 1, except that: the power of the applied alternating current is 240W, and the oxygen flow of the mass flow meter is regulated and controlled to be 80 sccm. In this example, the carbon peak in the X-ray spectrum is lower than that in example 1 due to the expansion of the oxygen flux and the reaction power, and the purity of the yttria in the product can be further improved.
Example 3
The preparation method is the same as that of example 1, except that: the precursor is prepared by mixing and grinding 0.5g of yttrium acetylacetonate and 0.025g of terbium acetylacetonate. In example 3, the peak position at 33 ° in XRD is slightly different from that of example 1 due to the difference in doping precursors.
Example 4
The preparation method is the same as that of example 1, except that: the precursor is prepared by mixing and grinding 0.5g of yttrium acetylacetonate and 0.05g of europium acetylacetonate, the alternating current power is 200W, and the treatment time is 20 min. The characteristic europium peak of the product obtained in example 4 is enhanced in the XRD pattern compared with that of example 1, and the lattice spacing of the TEM pattern differs from that of example 1.
The above examples are only for the purpose of clearly illustrating the process flow of the present invention. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, improvement and the like made by a person having ordinary skill in the art without departing from the principle of the present invention shall be included in the protection scope of the present invention.
Claims (10)
1. A method for preparing rare earth doped yttrium oxide fluorescent nanoparticles by a DBD technology, which is characterized by comprising the following steps:
(1) mixing the base metal organic matter and the doped metal organic matter according to the mass ratio of 10-40: 1, and grinding the mixture to be used as a reaction precursor;
(2) placing the precursor obtained in the step (1) in a container, wherein the container is placed between a positive electrode and a negative electrode of a plasma reactor;
(3) and then, applying alternating current between the cathode and the anode of the plasma reactor in an oxygen atmosphere, treating the precursor for a period of time, taking out products at intervals, and grinding to obtain the powder containing the rare earth doped yttrium oxide nanoparticles.
2. The method for preparing rare earth doped yttrium oxide fluorescent nanoparticles according to claim 1, wherein in the step (1), the agglomerated particles in the base metal organic and the doped metal organic are ground to a particle diameter of less than 0.2 mm.
3. The method for preparing rare earth doped yttrium oxide fluorescent nanoparticles according to claim 1 or 2, wherein in the step (1), the base metal organic is one or a combination of two or more of yttrium acetylacetonate, molybdenum cyclopentadienyl, yttrium hexafluoroacetylacetonate, molybdenum hexafluoroacetylacetonate, yttrium tris (2,2,6, 6-tetramethyl-3, 5-heptanedionate), and molybdenum tris (2,2,6, 6-tetramethyl-3, 5-heptanedionate).
4. The method for preparing rare earth-doped yttrium oxide fluorescent nanoparticles according to claim 1 or 2, wherein in the step (1), the doped metallorganics are europium acetylacetonate, terbium acetylacetonate, dysprosium acetylacetonate, thulium acetylacetonate, cerium acetylacetonate, praseodymium acetylacetonate, samarium acetylacetonate, europium tribasic, terbium tribasic, dysprosium tribasic, thulium tribasic, cerium tribasic, praseodymium tribasic, samarium hexafluoroacetylacetonate, terbium hexafluoroacetylacetonate, dysprosium hexafluoroacetylacetonate, thulium hexafluoroacetylacetonate, cerium hexafluoroacetylacetonate, praseodymium hexafluoroacetylacetonate, samarium hexafluoroacetylacetonate, europium tris (2,2,6, 6-tetramethyl-3, 5-heptanedionate), terbium tris (2,2,6, 6-tetramethyl-3, 5-heptanedionate) dysprosium, tris (2,2,6, 6-tetramethyl-3, 5-heptanedionate) thulium, tris (2,2,6, 6-tetramethyl-3, 5-heptanedionate) cerium, tris (2,2,6, 6-tetramethyl-3, 5-heptanedionate) praseodymium and tris (2,2,6, 6-tetramethyl-3, 5-heptanedionate) samarium.
5. The method for preparing rare earth doped yttrium oxide fluorescent nanoparticles according to claim 1 or 2, wherein in the step (2), the reaction precursor is placed in a quartz container, and the reaction precursor powder is paved at a position 2-3cm away from the center of the container; the top of the container is covered by a quartz plate with a size corresponding to the container.
6. The method for preparing rare earth doped yttrium oxide fluorescent nanoparticles according to claim 1 or 2, wherein in the step (2), the diameter of the stainless steel cathode cylinder of the plasma reactor is 50-70 mm, and the height is 15-30 mm; the anode and the cathode are the same in size; the distance between the cathode and the anode of the plasma reactor is 10-15 mm.
7. The method for preparing rare earth doped yttrium oxide fluorescent nanoparticles through the DBD technology as claimed in claim 1 or 2, wherein in the step (3), oxygen of 60-80 sccm is controlled and introduced into the container through a mass flow controller, and the oxygen is maintained until the reaction is completed, so that the oxygen atmosphere is ensured to exist all the time in the reaction process.
8. The method for preparing rare earth doped yttrium oxide fluorescent nanoparticles according to claim 1 or 2, wherein in the step (3), the applied alternating current ensures the output power to be 100-300W, so as to generate plasma between the positive and negative electrodes.
9. The method for preparing rare earth doped yttrium oxide fluorescent nanoparticles according to claim 1 or 2, wherein in the step (3), the precursor is treated for 5-30 min.
10. The method for preparing rare earth doped yttrium oxide fluorescent nanoparticles according to claim 1 or 2, wherein in the step (3), the product coated on the surface of the precursor is collected once every ten minutes and is fully ground to a nanometer shape with a particle size of 20-100 nm.
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