CN104726096A - Dysprosium-doped diindium trisulphide rare earth magnetic-fluorescent nano material and preparation method thereof - Google Patents
Dysprosium-doped diindium trisulphide rare earth magnetic-fluorescent nano material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a dysprosium-doped diindium trisulphide rare earth magnetic-fluorescent nano material and a preparation method thereof, and belongs to the technical field of nano materials. The molar content of dysprosium in the dysprosium-doped diindium trisulphide rare earth magnetic-fluorescent nano material is 0.773-2.590%. The preparation process comprises the following steps: preparing a to-be-reacted solution from an indium acetate solution, a dysprosium acetate solution, a mercaptoethanol solution and deionized water; carrying out gas-liquid contacting reaction on an atomized to-be-reacted solution and H2S gas carried by nitrogen; and treating a reaction product at 100 DEG C for 20 minutes to obtain the dysprosium-doped diindium trisulphide rare earth magnetic-fluorescent nano material. The dysprosium-doped diindium trisulphide rare earth magnetic-fluorescent nano material which is relatively strong in specific magnetism, relatively obvious in characteristic emission peak, uniform in particle and different in doping concentration is prepared by virtue of a liquid-gas chemical deposition method at room temperature.
Description
Technical field
The invention belongs to the technical field of nano material.Relate to and mix dysprosium indium trisulfide (In
2s
3dy
3+) adopt the inorganic liquid phase chemical deposition of spraying to prepare In under material and room temperature
2s
3dy
3+the method of magnetic-fluorescent multifunctional nano material.
Background technology
Rare earth nano material is an important branch in nano material, and the electron structure of rare earth element is rather special, and its out-shell electron forms about the same, and the 4f electronic shell of internal layer has unpaired electrons many especially.After rare earth material is prepared into Nano grade, because nano material possesses a series of specific responses such as surface-interface effect, macro quanta tunnel effect, quantum size effect, and the electronic structure of rare earth element uniqueness and larger atomic radius, thus make rare earth nano material have the performance of some excellences, have broad application prospects in fields such as fluorescent material, magneticsubstance, catalytic material, stupalith, thin-film materials.(1) fluorescent material field.Because rare earth element has unique spectral composition and excellent optical property, thus make rare earth nano material in fluorescent material, occupy very important deal.The optical property of rare earth element is mainly derived from the part forbidden transition jing of its electronics in 4f rail layer inside, and have following features: its emmission spectrum is wire, color clear, and fluorescent lifetime is long, high temperature resistant, excitation energy density is high.In addition rare earth nano fluorescent material is of a great variety, for giving numerous spectral informations, emission wavelength ranges wide (including from vacuum ultraviolet (VUV) near infrared spectral range), and part rare earth nano fluorescent material also has novel wavelength conversion characteristics, quantum-cutting effect and steady persistence effect.(2) field of magnetic material.In the crystal of rare earth metal, the shielding of outer 5s and 5p electronic shell is subject to during 4f layer electron synchrotron, so crystal field is more weak to the effect of 4f electronic orbit magnetic moment, even do not affect, the magnetic moment of atom of rare earth metal just includes 4f layer electronic orbit magnetic moment and the two-part contribution of spin magnetic moment in this case.Because in rare earth compound, 3d and 4f atoms metal magnetic moment all has contribution to the magnetic moment of compound, so its magnetic property is more excellent.The nano material of both magnetic and fluorescent dual-function has important application in chemistry, biology, medical field and biotechnology.
In
2s
3be a kind of N-type semiconductor, forbidden band is wide is 2.00 ~ 2.20eV, is typical III ~ VI family sulfide.It is the exotic materials with defect spinel structure, its each primitive unit cell is made up of octahedral and tetrahedral, all octahedral positions are all occupied by phosphide atom, and eight phosphide atoms occupy the position on tetrahedron, but on tetrahedral position, still there are four rooms.Because the existence in room makes In
2s
3a material of main part can be served as most of metal ion, there is the tendency of expulsion guest ions unlike other nano material.
At present, the preparation method of the rare earth nano material of report mainly contains template, sol-gel method, hydrothermal method, microemulsion method and the precipitator method.People (2009) the Bright white light emissionfromIn such as such as Anuja Datta
2s
3: Eu
3+nanoparticles.People (2013) the Hydrothermalsynthesis andluminescence properties ofYF such as Feng Tao
3: Ln (Ln=Sm, Dy, Tb and Pr) nano-/microcrystals.
Summary of the invention
The technical problem to be solved in the present invention is, a kind of method of more efficient deposition of rare-earth magnetic-fluorescent nano material under skilful use ultrasonic atomizatio method provides room temperature, synthesize saturation magnetization stronger, characteristic emission peak is comparatively obvious, the different levels of doping that granular size is homogeneous mix dysprosium indium trisulfide nano particulate material.
Resulting materials of the present invention mixes dysprosium indium trisulfide (In
2s
3dy
3+) rare-earth magnetic-fluorescent nano particle material.In
2s
3dy
3+the technical scheme of rare-earth magnetic-fluorescent nano particle material is:
One mixes dysprosium indium trisulfide rare-earth magnetic-fluorescent nano material, at In
2s
3dysprosium ion Some substitute indium ion in the structure of material; The molar content mixing dysprosium in dysprosium indium trisulfide rare-earth magnetic-fluorescent nano material is 0.773% ~ 2.590%.
For realizing object of the present invention, the concrete technical scheme that dysprosium indium trisulfide rare-earth magnetic-fluorescent nano material is mixed in the preparation of employing is:
Mix a preparation method for dysprosium indium trisulfide rare-earth magnetic-fluorescent nano material, have configuration question response solution, deposit the process of mixing dysprosium indium trisulfide nano material and aftertreatment; Described configuration question response solution, is indium acetate solution, acetic acid dysprosium solution and deionized water are mixed, and injects mercaptoethanol solution under whipped state; By acetic acid adjust ph 2.5 ~ 3.0, obtain question response solution; Wherein indium acetate, acetic acid dysprosium, mercaptoethanol and deionized water total amount are 1: 0.03 ~ 0.12: 1.0 ~ 1.5: 27000 ~ 28000 in molar ratio; Described deposition mixes dysprosium indium trisulfide nano material, is by the question response solution of atomization and the H carried with nitrogen
2s gas contacts in the reaction chamber, at 20 ~ 35 DEG C, liquid phases reaction occurs, and makes reaction product fall into collection device bottom reaction chamber; Wherein H
2the mol ratio of the indium ion in the total amount of S gas and question response liquid is 3 ~ 20: 1; Described aftertreatment, is that reaction product is processed 20 minutes, centrifugal extraction at 100 DEG C, then cleans 2-3 time respectively with deionized water and dehydrated alcohol, obtain mixing dysprosium indium trisulfide rare-earth magnetic-fluorescent nano material.
Described reaction chamber, can be concatenated into 2 ~ 3 grades, makes question response solution and the H of atomization
2s gas reaction is more abundant, by extending response path and time raising reaction efficiency.
Under described collection device can be in ultrasound environments, reunite to avoid reaction product.
Preferred indium acetate, acetic acid dysprosium, mercaptoethanol are 1: 0.03 ~ 0.06: 1.2 in molar ratio.What adopt this mol ratio to prepare mixes dysprosium indium trisulfide rare-earth magnetic-fluorescent nano material, has stronger magnetic function taking into account on fluorescent functional basis.
The question response solution of described atomization, can select the atomizing particle of 20 ~ 40 μm.
Na can be passed through in the lab
2s solution and excessive HCl solution reaction prepare H
2s gas.
The technical scheme that dysprosium indium trisulfide rare-earth magnetic-fluorescent nano material is mixed in laboratory preparation can be:
Experimental installation of the present invention is that combination builds, and is mainly divided into four parts: (1) produces reactant gases H
2the device of S; (2) device of ultrasonic atomizatio question response liquid; (3) there is main body reaction and the device of collecting reaction product; (4) exhaust gas processing device.As shown in Figure 1, specific experiment device is shown in embodiment 1.
First question response solution is configured: (1) is the indium acetate solution of 10mmol/L by the ionic concn that indium acetate and deionized water configure indium; Be the acetic acid dysprosium solution of 2mmol/L by the ion solubility of acetic acid dysprosium and deionized water configuration dysprosium; With the mercaptoethanol solution that mercaptoethanol and deionized water configuration concentration are 60mmol/L.(2) extract the indium acetate solution of 10mmol/L, the acetic acid dysprosium solution of 2mmol/L, deionized water mixing pour in clean beaker, and put into the stirrer that clean length is 2.5cm.Mixing solutions is placed on magnetic stirring apparatus, under whipped state, is slowly injected in the mixed solution of beaker with the mercaptoethanol solution that needle tubing extraction concentration is 60mmol/L, after stirring, makes it control between 2.5 ~ 3.0 by acetic acid adjust ph.
Then question response liquid is poured in ultrasonic atomizer, open prolong (reaction chamber) temperature-stable that circulator bath makes generation main body react at 25 DEG C; Open electromagnetic type air compressor pump, provide a negative pressure to whole reaction unit, make can pass into (the large I of fog is controlled by under meter) in reaction unit by the fog of question response solution (that is, being atomized reaction solution); Reactant gases H is produced in adjustment
2the setter of S device, allows Na in infusion bottle
2be equipped with below S solution is added dropwise in the there-necked flask of HCl solution.Open ultrasonic, pass into nitrogen, open ultrasonic atomizatio appliance mains switch.H under the carrying of nitrogen like this
2s gas just slowly can flow into three mouthfuls of pipe connectings, and contact with the atomization reaction solution that the other end from three mouthfuls of pipe connectings enters, afterwards first through the abundant hybrid reaction part of spherical condensation tube, then react fully through serpentine condenser, final reacting product drops in collection device Florence flask below, and the ultrasound environments at Florence flask place can avoid the reunion of reactant.A small amount of mixing fog that still unreacted is complete after above device can react through the serpentine condenser of another mouth again, and the reaction product generated is final also by the Florence flask that drops on below.Tail gas after series reaction device above passes into after the Erlenmeyer flask that NaOH is housed again through electromagnetic type air compressor pump, to reduce the corrosion to pump, the last tail gas bottle again passing into NaOH carries out absorbing unreacted atomizing gas, discharges after hydrogen sulfide through stink cupboard.
After reaction terminates, taken out by the Florence flask of collecting reaction product, being put into microwave power is in the MG08S-2B type microwave experiment instrument of 0 ~ 900W, carries out homogeneous heating, and setting heat-up time is 20min, and the temperature of heating is 100 DEG C.Finally reaction product is carried out centrifugal extraction, then clean 2 ~ 3 times respectively with deionized water and dehydrated alcohol.Sample after cleaning, can save as solid or liquid according to different requirements (such as test request).
Liquid phase of the present invention is the atomizing particle of 20 ~ 40 μm obtained with medical ultrasonic atomizer, used ultrasonic atomizatio method is a kind of method obtaining ultrafine particulate after being atomized by solution with physical means, its principle is when ultrasonic wave conduction arrives solution surface, liquid-gas interface ie in solution surface is in air interface and is subject to perpendicular to after interfacial hyperacoustic effect, due to hyperacoustic effect (i.e. energy), solution surface is made to form tensile wave, along with the enhancing of surface tension wave energy, when surface tension wave energy reaches certain value, also increase at the tensile wave crest of solution surface makes the liquid droplet at its crest place fly out simultaneously.Namely under hyperacoustic effect, utilize ultrasonic cavitation energy that a kind of solution transforms is become to have micro-misty liquid droplets of certain energy.
Effect of the present invention and feature:
(1) under the present invention room temperature, to prepare saturation magnetization comparatively strong for the method for liquid phase electroless plating, and characteristic emission peak is comparatively obvious, the different levels of doping that granular size is homogeneous mix dysprosium indium trisulfide nano particulate material.In nano material, small-size effect can cause the sound of material, optical, electrical, the characteristic such as magnetic, heat, mechanics changes, thus produces new physicals.Ingenious employing H in the present invention
2indium acetate is mixed dysprosium atomized particles and is surrounded by S gas, has easier obtained small size nano magnetic particle material.The aqueous phase synthesis methods for inorganic compounds of the liquids and gases reaction of this atomization, has more superiority than gas liquid reaction method in the past, makes reaction more abundant.
(2) magnetic-fluorescent dual-function rare-earth nanometer particles has nucleocapsid structure usually, namely on the core of magnetic nano-particle, directly rare earth nano fluorescent material is wrapped up, and rare earth ion of the present invention is the gained that directly adulterates, be prepare the another new methods of rare-earth magnetic-fluorescent nano material.After dysprosium ion mixes, dysprosium ion Some substitute indium ion, changes In
2s
3the structure of material, adds spin, has enriched the physical message of material.
(3) equipment of experiment is simply cheap, and reaction unit is built flexibly, according to reaction requirement, by adding the prolong of dissimilar number, can extend response path and time voluntarily, making reaction more fully controlled; The repeatability preparing sample is fine, is suitable for industrial mass production and uses.
Accompanying drawing explanation
Fig. 1 is the preparation In of use for laboratory of the present invention
2s
3dy
3+experimental installation sketch.
Fig. 2 is the In that the present invention is prepared by different ratios of raw materials
2s
3dy
3+the XRD figure spectrum of rare earth nano material.XRD figure spectrum and In
2s
3pdf card coincide
Fig. 3 is the In that example 3 obtains
2s
3dy
3+the High-Resolution Map of rare earth nano material.
Fig. 4 is the In that the present invention is prepared by different ratios of raw materials
2s
3dy
3+the M-H figure of rare earth nano material.
Fig. 5 is the In that the present invention is prepared by different ratios of raw materials
2s
3dy
3+the PL spectrogram of rare earth nano material.As can be seen from Figure 5, In
2s
3dy
3+dy is can be observed in fluorescence emission spectrogram under the excitation wavelength of nanoparticle 370nm excites
3+468nm, 482nm, 492nm characteristic emission peak, prove that Dy successfully mixes In
2s
3in.
Embodiment
Embodiment 1 composition graphs 1 illustrates that In is prepared in laboratory of the present invention
2s
3dy
3the apparatus structure of rare-earth magnetic-fluorescent nano material.
The present invention adopts the effective device of a kind of simple and flexible of building voluntarily to prepare rare earth nanometer particle material, as shown in Figure 1.
In Fig. 1, upper right portion is the first part of experimental installation: produce reactant gases H
2the device of S, main body is infusion bottle, transfusion device and there-necked flask, can by the setter on transfusion device, allows Na in infusion bottle
2s solution is equipped with in the there-necked flask of HCl solution below being added dropwise to the speed of per minute 16.The left side is the second section of experimental installation: device---the ultrasonic atomizer of ultrasonic atomizatio question response liquid, and question response liquid can be atomized into atomic little particle by it, can with H
2s is contact reacts more fully.Middle portion is the Part III of experimental installation: main body reaction occurs and the device of collecting reaction product, fog and H
2s gas is slowly flowed into by the two ends of three mouthfuls of pipe connectings and is fully contacted respectively, afterwards first through the abundant hybrid reaction part of spherical condensation tube, then react fully through serpentine condenser, final reacting product drops in collection device Florence flask below, a small amount of mixing fog that still unreacted is complete after above device can react through the serpentine condenser of another mouth again, the reaction product generated is final also by the Florence flask that drops on below, and the ultrasound environments at Florence flask place can avoid the reunion of reactant.The intake-outlet of serpentine condenser and spherical condensation tube is all connected with recirculated water, to control the temperature-stable of generation main body reaction at 25 DEG C.Lower right-most portion is the Part IV of experimental installation: exhaust gas processing device.Tail gas after series reaction device above passes into after the Erlenmeyer flask that NaOH is housed again through electromagnetic type air compressor pump, to reduce the corrosion to pump, the last tail gas bottle again passing into NaOH carries out absorbing unreacted atomizing gas, discharges after hydrogen sulfide through stink cupboard.
Embodiment 2 In
2s
3dy
3+the preparation (1) of rare-earth magnetic-fluorescent nano material
First question response solution is configured: the ionic concn configuring indium with indium acetate and deionized water is the solution of 10mmol/L; The ion solubility configuring dysprosium with acetic acid dysprosium and deionized water is the solution of 2mmol/L; Be the solution of 60mmol/L with mercaptoethanol and deionized water configuration concentration.Extraction indium ion solution 20mL, dysprosium ion solution 3mL, deionized water 73mL inject clean beaker, and put into the stirrer that clean length is 2.5cm.Mixing solutions is placed on magnetic stirring apparatus, under whipped state, extracts mercaptoethanol solution 4mL with needle tubing and be slowly injected in beaker, stir 30min, solution is mixed.Make it control between 2.5 ~ 3.0 by acetic acid adjust ph after stirring, configure question response liquid.Then question response liquid is poured in ultrasonic atomizer, by Na
2s and hydrochloric acid are poured in infusion bottle and there-necked flask respectively.The H that hydrochloric acid and sodium sulphite reaction generate
2indium ion (In in the total amount of S gas and question response liquid
3+) mol ratio be 3 ~ 20:1 (H
2s gas is excessive).Open prolong temperature-stable that circulator bath makes generation main body react at 25 DEG C, open the ultrasound environments of collecting reaction product, open electromagnetic type air compressing pumping source.Open nitrogen pressure valve, produce H
2s gas, adjust flux setter makes Na
2the speed of S solution drips is per minute 16.Under the carrying of nitrogen, H
2s gas slowly flows in reaction chamber.Open ultrasonic atomizer, be transferred to maximum atomization quantity, the reaction solution of atomization enter in reaction chamber with H
2s gas fully reacts, and reacts sustainable 10 ~ 12 hours.
After reaction terminates, taken out by the Florence flask of collecting reaction product, being put into microwave power is in the MG08S-2B type microwave experiment instrument of 0-900W, carries out homogeneous heating, and setting heat-up time is 20min, and the temperature of heating is 100 DEG C.Finally reaction product is carried out centrifugal extraction, then clean 2 ~ 3 times respectively with deionized water and dehydrated alcohol.Sample after cleaning, can save as solid or liquid according to different requirements.
According to the test of transmission electron microscope power spectrum, last In
2s
3dy
3+in rare-earth magnetic-fluorescent nano material product, the molar content of dysprosium is 0.773%.Obtained In
2s
3dy
3+the XRD figure spectrum of rare earth nano material particle is shown in Fig. 2, and M-H curve is shown in Fig. 4, and PL spectrogram is shown in Fig. 5.In figure 3% represents that in reaction solution, the molar weight of dysprosium ion is 3: 100 with the ratio of the molar weight of indium ion.
Embodiment 3 In
2s
3dy
3+the preparation (2) of rare-earth magnetic-fluorescent nano material
First question response solution is configured: the ionic concn configuring indium with indium acetate and deionized water is the solution of 10mmol/L; The ion solubility configuring dysprosium with acetic acid dysprosium and deionized water is the solution of 2mmol/L; Be the solution of 60mmol/L with mercaptoethanol and deionized water configuration concentration.Extraction indium ion solution 20mL, dysprosium ion solution 6mL, deionized water 70mL inject clean beaker, and put into the stirrer that clean length is 2.5cm.Mixing solutions is placed on magnetic stirring apparatus, under whipped state, extracts mercaptoethanol solution 4mL with needle tubing and be slowly injected in beaker, stir 30min, solution is mixed.Make it control between 2.5 ~ 3.0 by acetic acid adjust ph after stirring, configure question response liquid.Then question response liquid is poured in ultrasonic atomizer, by Na
2s and hydrochloric acid are poured in infusion bottle and there-necked flask respectively.The H that hydrochloric acid and sodium sulphite reaction generate
2indium ion (In in the total amount of S gas and question response liquid
3+) mol ratio be 3 ~ 20:1 (H
2s gas is excessive).Open prolong temperature-stable that circulator bath makes generation main body react at 25 DEG C, open the ultrasound environments of collecting reaction product, open electromagnetic type air compressing pumping source.Open nitrogen pressure valve, produce H
2s gas, adjust flux setter makes Na
2the speed of S solution drips is per minute 16.Under the carrying of nitrogen, H
2s gas slowly flows in reaction chamber.Open ultrasonic atomizer, be transferred to maximum atomization quantity, the reaction solution of atomization enter in reaction chamber with H
2s gas fully reacts, and reacts sustainable 10 ~ 12 hours.
After reaction terminates, taken out by the Florence flask of collecting reaction product, being put into microwave power is in the MG08S-2B type microwave experiment instrument of 0-900W, carries out homogeneous heating, and setting heat-up time is 20min, and the temperature of heating is 100 DEG C.Finally reaction product is carried out centrifugal extraction, then clean 2 ~ 3 times respectively with deionized water and dehydrated alcohol.Sample after cleaning, can save as solid or liquid according to different requirements.
According to the test of transmission electron microscope power spectrum, last In
2s
3dy
3+in rare-earth magnetic-fluorescent nano material product, the molar content of dysprosium is 1.365%.Obtained In
2s
3dy
3+the XRD figure spectrum of rare earth nano material particle is shown in Fig. 2, and M-H curve is shown in Fig. 4, and PL spectrogram is shown in Fig. 5.In figure 6% represents that in reaction solution, the molar weight of dysprosium ion is 6: 100 with the ratio of the molar weight of indium ion.
Embodiment 4 In
2s
3dy
3+the preparation (3) of rare-earth magnetic-fluorescent nano material
First question response solution is configured: the ionic concn configuring indium with indium acetate and deionized water is the solution of 10mmol/L; The ion solubility configuring dysprosium with acetic acid dysprosium and deionized water is the solution of 2mmol/L; Be the solution of 60mmol/L with mercaptoethanol and deionized water configuration concentration.Extraction indium ion solution 20mL, dysprosium ion solution 9mL, deionized water 67mL inject clean beaker, and put into the stirrer that clean length is 2.5cm.Mixing solutions is placed on magnetic stirring apparatus, under whipped state, extracts mercaptoethanol solution 4mL with needle tubing and be slowly injected in beaker, stir 30min, solution is mixed.Make it control between 2.5 ~ 3.0 by acetic acid adjust ph after stirring, configure question response liquid.Then question response liquid is poured in ultrasonic atomizer, by Na
2s and hydrochloric acid are poured in infusion bottle and there-necked flask respectively.The H that hydrochloric acid and sodium sulphite reaction generate
2indium ion (In in the total amount of S gas and question response liquid
3+) mol ratio be 3 ~ 20:1.Open prolong temperature-stable that circulator bath makes generation main body react at 25 DEG C, open the ultrasound environments of collecting reaction product, open electromagnetic type air compressing pumping source.Open nitrogen pressure valve, produce H
2s gas, adjust flux setter makes Na
2the speed of S solution drips is per minute 16.Under the carrying of nitrogen, H
2s gas slowly flows into (H in reaction chamber
2s gas usage is excessive relative to indium ion).Open ultrasonic atomizer, be transferred to maximum atomization quantity, the reaction solution of atomization enter in reaction chamber with H
2s gas fully reacts, and reacts sustainable 10 ~ 12 hours.
After reaction terminates, taken out by the Florence flask of collecting reaction product, being put into microwave power is in the MG08S-2B type microwave experiment instrument of 0-900W, carries out homogeneous heating, and setting heat-up time is 20min, and the temperature of heating is 100 DEG C.Finally reaction product is carried out centrifugal extraction, then clean 2 ~ 3 times respectively with deionized water and dehydrated alcohol.Sample after cleaning, can save as solid or liquid according to different requirements.
According to the test of transmission electron microscope power spectrum, last In
2s
3dy
3+in rare-earth magnetic-fluorescent nano material product, the molar content of dysprosium is 2.590%.Obtained In
2s
3dy
3+the XRD figure spectrum of rare earth nano material particle is shown in Fig. 2, and M-H curve is shown in Fig. 4, and PL spectrogram is shown in Fig. 5.In figure 9% represents that in reaction solution, the molar weight of dysprosium ion is 9: 100 with the ratio of the molar weight of indium ion.
Embodiment 5 In
2s
3dy
3+the preparation (4) of rare-earth magnetic-fluorescent nano material
First question response solution is configured: the ionic concn configuring indium with indium acetate and deionized water is the solution of 10mmol/L; The ion solubility configuring dysprosium with acetic acid dysprosium and deionized water is the solution of 2mmol/L; Be the solution of 60mmol/L with mercaptoethanol and deionized water configuration concentration.Extraction indium ion solution 20mL, dysprosium ion solution 12mL, deionized water 64mL inject clean beaker, and put into the stirrer that clean length is 2.5cm.Mixing solutions is placed on magnetic stirring apparatus, under whipped state, extracts mercaptoethanol solution 4mL with needle tubing and be slowly injected in beaker, stir 30min, solution is mixed.Make it control between 2.5 ~ 3.0 by acetic acid adjust ph after stirring, configure question response liquid.Then question response liquid is poured in ultrasonic atomizer, by Na
2s and hydrochloric acid are poured in infusion bottle and there-necked flask respectively.Open prolong temperature-stable that circulator bath makes generation main body react at 25 DEG C, open the ultrasound environments of collecting reaction product, open electromagnetic type air compressing pumping source.Open nitrogen pressure valve, produce H
2s gas, adjust flux setter makes Na
2the speed of S solution drips is per minute 16.Under the carrying of nitrogen, H
2s gas slowly flows into (H in reaction chamber
2s gas usage is excessive relative to indium ion).Open ultrasonic atomizer, be transferred to maximum atomization quantity, the reaction solution of atomization enter in reaction chamber with H
2s gas fully reacts, and reacts sustainable 10 ~ 12 hours.
After reaction terminates, taken out by the Florence flask of collecting reaction product, being put into microwave power is in the MG08S-2B type microwave experiment instrument of 0-900W, carries out homogeneous heating, and setting heat-up time is 20min, and the temperature of heating is 100 DEG C.Finally reaction product is carried out centrifugal extraction, then clean 2 ~ 3 times respectively with deionized water and dehydrated alcohol.Sample after cleaning, can save as solid or liquid according to different requirements.
According to the test of transmission electron microscope power spectrum, in last In2S3Dy3+ rare-earth magnetic-fluorescent nano material product, the molar content of dysprosium is 1.180%.The XRD figure spectrum of obtained In2S3Dy3+ rare earth nano material particle is shown in Fig. 2, and M-H curve is shown in Fig. 4, and PL spectrogram is shown in Fig. 5.In figure 12% represents that in reaction solution, the molar weight of dysprosium ion is 12: 100 with the ratio of the molar weight of indium ion.
Claims (6)
1. mix dysprosium indium trisulfide rare-earth magnetic-fluorescent nano material, it is characterized in that, at In
2s
3dysprosium ion Some substitute indium ion in the structure of material; The molar content mixing dysprosium in dysprosium indium trisulfide rare-earth magnetic-fluorescent nano material is 0.773% ~ 2.590%.
2. the preparation method mixing dysprosium indium trisulfide rare-earth magnetic-fluorescent nano material of claim 1, has configuration question response solution, deposits the process of mixing dysprosium indium trisulfide nano material and aftertreatment; Described configuration question response solution, is indium acetate solution, acetic acid dysprosium solution and deionized water are mixed, and injects mercaptoethanol solution under whipped state; By acetic acid adjust ph 2.5 ~ 3.0, obtain question response solution; Wherein indium acetate, acetic acid dysprosium, mercaptoethanol and deionized water total amount are 1: 0.03 ~ 0.12: 1.0 ~ 1.5: 27000 ~ 28000 in molar ratio; Described deposition mixes dysprosium indium trisulfide nano material, is by the question response solution of atomization and the H carried with nitrogen
2s gas contacts in the reaction chamber, at 20 ~ 35 DEG C, liquid phases reaction occurs, and makes reaction product fall into collection device bottom reaction chamber; Wherein H
2the mol ratio of the indium ion in the total amount of S gas and question response liquid is 3 ~ 20: 1; Described aftertreatment, is that reaction product is processed 20 minutes, centrifugal extraction at 100 DEG C, then cleans 2 ~ 3 times respectively with deionized water and dehydrated alcohol, obtain mixing dysprosium indium trisulfide rare-earth magnetic-fluorescent nano material.
3. the preparation method mixing dysprosium indium trisulfide rare-earth magnetic-fluorescent nano material according to claim 2, is characterized in that, described reaction chamber is concatenated into 2 ~ 3 grades.
4. the preparation method mixing dysprosium indium trisulfide rare-earth magnetic-fluorescent nano material according to Claims 2 or 3, is characterized in that, under described collection device is in ultrasound environments, reunites to avoid reaction product.
5. the preparation method mixing dysprosium indium trisulfide rare-earth magnetic-fluorescent nano material according to Claims 2 or 3, is characterized in that, indium acetate, acetic acid dysprosium, mercaptoethanol are 1: 0.03 ~ 0.06: 1.2 in molar ratio.
6. the preparation method mixing dysprosium indium trisulfide rare-earth magnetic-fluorescent nano material according to claim 2, is characterized in that, the question response solution of described atomization, selects the atomizing particle of 20 ~ 40 μm.
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|---|---|---|---|---|
| CN109943338A (en) * | 2019-03-18 | 2019-06-28 | 中国计量大学 | A kind of near-infrared luminous rear-earth-doped InSe nanometer piece preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109943338A (en) * | 2019-03-18 | 2019-06-28 | 中国计量大学 | A kind of near-infrared luminous rear-earth-doped InSe nanometer piece preparation method |
| CN109943338B (en) * | 2019-03-18 | 2021-12-28 | 中国计量大学 | Preparation method of near-infrared luminescent rare earth doped indium selenide nanosheet |
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