CN113247958A - Magnetic fluorescent nano composite material and preparation method and application thereof - Google Patents
Magnetic fluorescent nano composite material and preparation method and application thereof Download PDFInfo
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- 239000002114 nanocomposite Substances 0.000 title claims abstract description 48
- 239000000463 material Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000002105 nanoparticle Substances 0.000 claims abstract description 60
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 30
- 239000012498 ultrapure water Substances 0.000 claims abstract description 30
- 229910015667 MoO4 Inorganic materials 0.000 claims abstract description 28
- 229960002089 ferrous chloride Drugs 0.000 claims abstract description 26
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims abstract description 26
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract description 24
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 23
- 238000002156 mixing Methods 0.000 claims abstract description 20
- -1 rare earth ions Chemical class 0.000 claims abstract description 18
- 238000001514 detection method Methods 0.000 claims abstract description 14
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 14
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000000975 co-precipitation Methods 0.000 claims abstract description 6
- 229910052693 Europium Inorganic materials 0.000 claims abstract description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 3
- 239000011733 molybdenum Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 68
- 238000010438 heat treatment Methods 0.000 claims description 35
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 25
- 239000011259 mixed solution Substances 0.000 claims description 25
- 229940032296 ferric chloride Drugs 0.000 claims description 23
- 239000000203 mixture Substances 0.000 claims description 23
- 238000003756 stirring Methods 0.000 claims description 23
- 238000005303 weighing Methods 0.000 claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 19
- 239000002244 precipitate Substances 0.000 claims description 19
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 16
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 229910017604 nitric acid Inorganic materials 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 15
- 229910001940 europium oxide Inorganic materials 0.000 claims description 12
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 claims description 12
- 229920002873 Polyethylenimine Polymers 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 10
- 239000001509 sodium citrate Substances 0.000 claims description 10
- 239000011684 sodium molybdate Substances 0.000 claims description 10
- 235000015393 sodium molybdate Nutrition 0.000 claims description 10
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 10
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims description 10
- 229940038773 trisodium citrate Drugs 0.000 claims description 10
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 9
- 238000001704 evaporation Methods 0.000 claims description 8
- 238000003760 magnetic stirring Methods 0.000 claims description 7
- 229910002651 NO3 Inorganic materials 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 6
- 239000000376 reactant Substances 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 2
- 229940044631 ferric chloride hexahydrate Drugs 0.000 claims description 2
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- 239000002122 magnetic nanoparticle Substances 0.000 claims description 2
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000009776 industrial production Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 230000035945 sensitivity Effects 0.000 abstract description 3
- 239000002351 wastewater Substances 0.000 abstract description 3
- 230000005684 electric field Effects 0.000 abstract 1
- CZMAIROVPAYCMU-UHFFFAOYSA-N lanthanum(3+) Chemical compound [La+3] CZMAIROVPAYCMU-UHFFFAOYSA-N 0.000 abstract 1
- 231100000053 low toxicity Toxicity 0.000 abstract 1
- 238000010189 synthetic method Methods 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 13
- 238000009826 distribution Methods 0.000 description 8
- GAGGCOKRLXYWIV-UHFFFAOYSA-N europium(3+);trinitrate Chemical compound [Eu+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O GAGGCOKRLXYWIV-UHFFFAOYSA-N 0.000 description 8
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 8
- 238000012423 maintenance Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000012544 monitoring process Methods 0.000 description 5
- 230000008859 change Effects 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 230000005389 magnetism Effects 0.000 description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 238000004020 luminiscence type Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000001808 coupling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- RSEIMSPAXMNYFJ-UHFFFAOYSA-N europium(III) oxide Inorganic materials O=[Eu]O[Eu]=O RSEIMSPAXMNYFJ-UHFFFAOYSA-N 0.000 description 1
- 229960004887 ferric hydroxide Drugs 0.000 description 1
- 239000012456 homogeneous solution Substances 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 description 1
- 229910021506 iron(II) hydroxide Inorganic materials 0.000 description 1
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000004297 night vision Effects 0.000 description 1
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide [Fe3O4]
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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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/006—Compounds containing, besides molybdenum, two or more other elements, with the exception of oxygen or hydrogen
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
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- 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
- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
- C09K11/7794—Vanadates; Chromates; Molybdates; Tungstates
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R31/00—Arrangements for testing electric properties; Arrangements for locating electric faults; Arrangements for electrical testing characterised by what is being tested not provided for elsewhere
- G01R31/50—Testing of electric apparatus, lines, cables or components for short-circuits, continuity, leakage current or incorrect line connections
- G01R31/52—Testing for short-circuits, leakage current or ground faults
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Abstract
The invention discloses a magnetic fluorescent nano composite material and a preparation method and application thereof, wherein the preparation method comprises the step of preparing magnetic Fe by using ferric chloride and ferrous chloride through a coprecipitation method3O4The nano-particles, two-purpose three rare earth ions of lanthanum ion, europium ion and molybdenum ion are used for preparing La by a hydrothermal method2(MoO4)3:Eu3+Fluorescent nano-particles, namely adding La2(MoO4)3: Eu3+ fluorescent nano-particles and magnetic Fe3O4 nano-particles into ultrapure water or absolute ethyl alcohol in proportion by a three-way blending method to blend into a magnetic fluorescent nano-composite material; after a circuit is short-circuited, the magnetic fluorescent nano composite material can instantly generate an electric field, so that the detection sensitivity is effectively enhanced, the indication time of a display is improved, and the fault detection efficiency is improved; the synthetic method is simple and environment-friendly, has few raw material types, low toxicity and little waste water, and is suitable for industrial production; after the fault indicator is applied to the fault indicator, the working intensity of personnel can be reduced, the working efficiency is improved, the personnel are assisted to explore power grid accidents in time, and the power grid safety is maintained.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a magnetic fluorescent nano composite material, and a preparation method and application thereof.
Background
The fault indicator is a key component of power distribution facilities in a power system, and mainly has the functions of timely detecting a power fault location and shortening the fault power failure range and time. With the rapid development of socio-economy, people have higher and higher requirements on the reliability of power supply. At present, the daily routing inspection mode of the power distribution network fault detector is still relatively lagged behind, and a method of matching a device type instrument, an active online fault positioning system and a manual routing inspection mode is mainly adopted.
However, most of the devices need active power for driving, the device is relatively complex and has many limitations, and the line selection is only suitable for small current and is easy to break down under the high-voltage and high-current environment; meanwhile, the operation, equipment, security and protection of different fault detectors and the monitoring content of an environment monitoring system are different under the limitation of objective conditions; moreover, as the fault detectors are multiple in points and wide in range, and the number of operation and maintenance personnel of the distribution network of a power supply enterprise is seriously insufficient, the labor intensity of the personnel of the distribution network at the basic level is extremely high, and the timely exploration of power grid accidents and the safe maintenance of the power grid are difficult to ensure; in order to solve the above problems, it is necessary to develop a magnetic fluorescent nanocomposite material, and a method for preparing and using the same.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a magnetic fluorescent nano composite material and a preparation method and application thereof, wherein the magnetic fluorescent nano composite material can instantaneously induce the change of a magnetic field after a circuit is short-circuited, effectively enhances the detection sensitivity of a fault detection and acquisition system, improves the indication time of a display, greatly improves the fault detection efficiency, and assists the fault detection system to achieve the purposes of rapid, efficient and intelligent detection and monitoring; the synthesis method is simpler and more environment-friendly, the variety of the required raw materials is less, the toxicity is low, the generated wastewater is less, and the method is suitable for industrial production; after the fault indicator is applied to the fault indicator, the working strength of distribution network operation and maintenance personnel can be reduced, the working efficiency is improved, the distribution network operation and maintenance personnel are assisted to probe power grid accidents in time, and the power grid safety is maintained.
The purpose of the invention is realized as follows: in a first aspect, a method for preparing a magnetic fluorescent nanocomposite material is provided, which comprises the following steps:
(1) preparing magnetic nanoparticles: magnetic Fe is prepared by adopting ferric chloride and ferrous chloride through a coprecipitation method3O4 nanoparticles;
(2) preparing fluorescent nanoparticles: la is prepared by three rare earth ions through a hydrothermal method2(MoO4)3:Eu3+Fluorescent nanoparticles, wherein three rare earth ions are respectively lanthanum ions, europium ions and molybdenum ions;
(3) preparing a magnetic fluorescent nano composite material: mixing La2(MoO4)3:Eu3+Fluorescent nanoparticles and magnetic Fe3O4The nano particles are added into ultrapure water or absolute ethyl alcohol according to a certain proportion and blended to obtain the magnetic fluorescent nano composite material.
Method for preparing a preferred magnetic fluorescent nanocomposite, said magnetic Fe3O4The preparation of the nano-particles comprises the following steps:
step one, adding ferric chloride and ferrous chloride into deionized water according to a certain proportion, heating, and stirring to completely dissolve the ferric chloride and the ferrous chloride to obtain an orange uniform solution;
adding a sodium hydroxide solution or ammonia water into the solution, and adjusting the pH value of the solution; wherein, sodium hydroxide and ammonia water are used as precipitating agents and respectively react with ferric chloride and ferrous chloride to produce ferric hydroxide and ferrous hydroxide precipitate;
adding trisodium citrate into the solution, heating, continuing stirring, filtering, and centrifugally washing the filtrate for multiple times by using ultrapure water; wherein the carboxyl group in trisodium citrate can react with Fe3O4The surface action forms an organic film which is dispersed by static electricity and smaller steric hindrance, so that Fe3O4The particles do not agglomerate, thereby obtaining nanoparticles;
step four, drying the filtered substances which are washed for many times at high temperature to obtain magnetic Fe3O4And (3) nanoparticles.
In the step one, 0.6-2.23 g of ferric chloride, 0.3-1.14 g of ferrous chloride and 30ml of deionized water are added, the heating and stirring temperature is 50-70 ℃, and the heating and stirring time is 20-40 minutes;
in the second step, the pH value of the solution is controlled to be 9-11;
in the third step, 0.2-0.3 g of trisodium citrate is added, the temperature is raised to 70-90 ℃, and the mixture is heated and stirred for 50-70 minutes;
in the fourth step, the high-temperature drying temperature is 110-130 ℃, and the high-temperature drying time is 2-3 hours.
So far, the chemical coprecipitation method provided by the invention is used for preparing the nano magnetic Fe3O4Mixing ferrous salt solution and ferric salt solution according to a certain proportion, adding excessive alkaline precipitator into the ferric salt mixed solution, stirring at a high speed for reaction for a period of time under a certain PH value, adding trisodium citrate during the reaction to improve the dispersion property, and finally centrifuging, washing and drying to obtain the nano magnetic Fe3O4Particles whose reaction principle is as follows:
Fe2+＋2Fe3+＋8OH-→Fe3O4＋4H2O。
in the preferred preparation method of the magnetic fluorescent nano composite material, ferric chloride hexahydrate can be adopted as the ferric chloride, and ferrous chloride tetrahydrate can be adopted as the ferrous chloride.
A preferred method for preparing a magnetic fluorescent nanocomposite, said La2(MoO4)3:Eu3+The preparation of the fluorescent nanoparticles comprises the following steps:
firstly, weighing lanthanum oxide and europium oxide according to a proportion, uniformly mixing, adding concentrated nitric acid, heating to dissolve rare earth oxide, and evaporating redundant concentrated nitric acid to dryness to obtain white powdery rare earth nitrate;
dissolving white powdery rare earth nitrate in ultrapure water, adding a polyethyleneimine solution, and uniformly mixing to form a solution A; wherein, the polyethyleneimine solution is a surfactant, and the coupling effect and the reactivity of the surfactant are utilized to prepare the nano-particles;
weighing sodium molybdate according to a proportion, dissolving the sodium molybdate with ultrapure water to form a solution B, quickly injecting the solution B into the solution A under magnetic stirring, adding ammonia water into the mixed solution, adjusting the pH value of the mixed solution, and continuing stirring; wherein, the magnetic stirring is adopted to achieve the purpose of rapid and uniform mixing;
transferring the mixed solution into a hydrothermal reaction kettle, sealing, reacting at a certain temperature for a certain time, unsealing after the reaction kettle is cooled to room temperature, centrifugally separating reactants to obtain white precipitates, washing the white precipitates with ultrapure water and absolute ethyl alcohol for multiple times respectively, and fully drying the precipitates after washing for multiple times in a constant-temperature oven to obtain La2(MoO4)3:Eu3+Fluorescent nanoparticles.
In the step one, the mass of added lanthanum oxide is 0.3-1.14 g, the mass of europium oxide is 0.2-0.53 g, the heating and dissolving temperature is 40-60 ℃, and the evaporation temperature is 80-90 ℃;
in the second step, the concentration of the added polyethyleneimine solution is 99%, and the volume of the added polyethyleneimine solution is 1-5 ml;
in the third step, 1.21-3.63 g of sodium molybdate is added, the pH value of the mixed solution is controlled to be 8-12, and the mixture is continuously stirred for 10-15 minutes;
in the fourth step, the reaction temperature after the hydrothermal reaction kettle is sealed is 140-170 ℃, the reaction time is 5-8 hours, and the constant temperature drying temperature is 60-80 ℃.
So far, the hydrothermal method provided by the invention is used for preparing La2(MoO4)3:Eu3+Of fluorescent nanoparticlesIn the process, the chemical reaction formula is as follows:
La2O3+6HNO3=2La(NO3)3+3H2O；
Eu2O3+6HNO3=2Eu(NO3)3+3H2O；
MoO4 2++ La3++ Eu=La2(MoO4)3:Eu3+。
preparation method of preferred magnetic fluorescent nano composite material, and in blending, La is adopted2(MoO4)3:Eu3+Fluorescent nanoparticles and said magnetic Fe3O4The addition ratio of the nanoparticles is 1: 3-5: 1.
In a second aspect, a magnetic fluorescent nanocomposite material is provided, which is prepared according to the preparation method of any one of the first aspect.
In a third aspect, the application of the magnetic fluorescent nanocomposite material is provided, and the magnetic fluorescent nanocomposite material is applied to a fault indicator in the field of electric power detection.
Due to the adoption of the technical scheme, the invention has the beneficial effects that:
(1) the magnetic fluorescent nano composite material can instantly induce the change of a magnetic field after a circuit is short-circuited, so that magnetic red particles in a solution are disturbed and dispersed, the whole solution can rapidly display obvious red color and is easy to identify, the night vision color development function of a display is enhanced, the detection sensitivity of a fault detection and acquisition system is effectively enhanced, the indication time of the display is prolonged, the fault detection efficiency is greatly improved, and the fault detection system is assisted to achieve the purposes of rapid, efficient and intelligent detection and monitoring;
(2) the invention adopts coprecipitation method to synthesize magnetic Fe3O4Nano particles, synthesizing La by hydrothermal method2(MoO4)3:Eu3 +The fluorescent nano-particles are synthesized into the magnetic fluorescent nano-composite material by adopting a blending method, the synthesis method is simpler and more environment-friendly, the variety of the required raw materials is less, the toxicity is low,the generated wastewater is less, and the method is suitable for industrial production;
(3) after the fault indicator is applied to the fault indicator, the working intensity of distribution network operation and maintenance personnel can be reduced, the working efficiency is improved, the distribution network operation and maintenance personnel are assisted to explore power grid accidents in time, and the power grid safety is maintained.
Drawings
FIG. 1 is a graph showing the results of a luminescence coloration test (irradiation with a 365nm wavelength laser) of the magnetic fluorescent nanocomposite obtained in example 1 of the present invention.
FIG. 2 is a graph showing the results of particle size measurements on the magnetic fluorescent nanocomposites obtained in example 2 of the present invention in various ratios.
FIG. 3 is a graph showing the results of fluorescence intensity measurements on magnetic fluorescent nanocomposites obtained in example 3 of the present invention in various ratios.
FIG. 4 shows the magnetic fluorescent nanocomposite obtained in example 4 of the present invention and pure magnetic Fe3O4And (4) a hysteresis loop test comparison result chart of the nano particles.
Detailed Description
The technical scheme of the invention is further specifically described by the following embodiments.
Example 1
Magnetic Fe3O4Preparing nano particles: weighing 30ml of deionized water, adding the deionized water into a 100ml beaker, weighing 0.6g of ferric chloride and 0.3g of ferrous chloride, adding the ferric chloride and the ferrous chloride into the beaker, heating the mixture at the temperature of 50 ℃, and stirring the mixture for 40 minutes to completely dissolve the ferric chloride and the ferrous chloride to obtain an orange uniform solution; adding sodium hydroxide solution to the solution, and adjusting the pH = 9; adding 0.2g trisodium citrate into the solution, heating to 70 deg.C, stirring for 70 min, stopping heating, and filtering to obtain Fe (OH)2And Fe (OH)3Filtering the mixture; centrifugally washing the filtrate with ultrapure water for three times, and drying at 110 deg.C for 3 hr to obtain magnetic Fe3O4And (3) nanoparticles.
La2(MoO4)3:Eu3+Preparing fluorescent nanoparticles: an appropriate amount of concentrated nitric acid (concentration 68%) is measured and added into a 100ml beakerWeighing 0.3g of lanthanum oxide and 0.2g of europium oxide, uniformly mixing, adding into a beaker, heating to 40 ℃, heating to 80 ℃ after the lanthanum oxide and the europium oxide are completely dissolved, and evaporating redundant concentrated nitric acid to obtain white powdery lanthanum nitrate and europium nitrate; dissolving white powdery lanthanum nitrate and europium nitrate in a proper amount of ultrapure water, adding 1ml of 99% polyethyleneimine solution, and uniformly mixing to form a solution A; weighing 1.21g of sodium molybdate, and dissolving with a proper amount of ultrapure water to form a solution B; under magnetic stirring, quickly injecting the solution B into the solution A to form a mixed solution; adding ammonia water into the mixed solution, adjusting the pH =8, and then continuing stirring for 10 minutes; then transferring the mixed solution into a hydrothermal reaction kettle, sealing and reacting the mixed solution at 140 ℃ for 8 hours; after the reaction kettle is cooled to room temperature, unsealing, and centrifugally separating reactants to obtain a white precipitate; washing the white precipitate with ultrapure water and absolute ethyl alcohol for three times respectively, and then putting the washed white precipitate into a constant-temperature oven at 60 ℃ for full drying to obtain La2(MoO4)3:Eu3+Fluorescent nanoparticles.
Preparing a magnetic fluorescent nano composite material: subjecting the obtained La to2(MoO4)3:Eu3+Fluorescent nanoparticles and magnetic Fe3O4The nanometer particles are added into a proper amount of ultrapure water according to the proportion of 1:3, 1:2, 1:1, 1.5:1, 2:1, 2.5:1, 3:1, 4:1 and 5:1, and are blended to form the magnetic fluorescent nanometer composite material.
Example 2
Magnetic Fe3O4Preparing nano particles: weighing 30ml of deionized water, adding the deionized water into a 100ml beaker, weighing 1.14g of ferric chloride and 0.58g of ferrous chloride, adding the ferric chloride and the ferrous chloride into the beaker, heating the mixture at the temperature of 60 ℃, and stirring the mixture for 30 minutes to completely dissolve the ferric chloride and the ferrous chloride to obtain an orange uniform solution; adding sodium hydroxide solution to the solution, adjusting PH = 9.5; adding 0.23g trisodium citrate into the solution, heating to 80 deg.C, heating and stirring for 60 min, stopping heating, and filtering the reaction solution to obtain Fe (OH)2And Fe (OH)3Filtering the mixture; centrifugally washing the filtrate with ultrapure water for three times, and drying at 120 deg.C for 2.5 hr to obtain magnetic Fe3O4And (3) nanoparticles.
La2(MoO4)3:Eu3+Preparing fluorescent nanoparticles: weighing a proper amount of concentrated nitric acid (with the concentration of 68%) and adding the concentrated nitric acid into a 100ml beaker, weighing 0.58g of lanthanum oxide and 0.31g of europium oxide, uniformly mixing, adding the mixture into the beaker, heating the mixture to the temperature of 50 ℃, heating the mixture to 85 ℃ after the lanthanum oxide and the europium oxide are completely dissolved, and evaporating redundant concentrated nitric acid to obtain white powdery lanthanum nitrate and europium nitrate; dissolving white powdery lanthanum nitrate and europium nitrate with a proper amount of ultrapure water, adding 2.4ml of 99% polyethyleneimine solution, and uniformly mixing to form a solution A; weighing 2.01g of sodium molybdate, and dissolving with a proper amount of ultrapure water to form a solution B; under magnetic stirring, quickly injecting the solution B into the solution A to form a mixed solution; adding ammonia water into the mixed solution, adjusting the pH =9, and then continuing stirring for 10 minutes; then transferring the mixed solution into a hydrothermal reaction kettle, sealing and reacting the mixed solution at 150 ℃ for 7 hours; after the reaction kettle is cooled to room temperature, unsealing, and centrifugally separating reactants to obtain a white precipitate; washing the white precipitate with ultrapure water and absolute ethyl alcohol for three times respectively, and then putting the washed white precipitate into a constant-temperature oven at 70 ℃ for full drying to obtain La2(MoO4)3:Eu3+Fluorescent nanoparticles.
Preparing a magnetic fluorescent nano composite material: subjecting the obtained La to2(MoO4)3:Eu3+Fluorescent nanoparticles and magnetic Fe3O4The nanometer particles are added into a proper amount of ultrapure water according to the proportion of 1:3, 1:2, 1:1, 1.5:1, 2:1, 2.5:1, 3:1, 4:1 and 5:1, and are blended to form the magnetic fluorescent nanometer composite material.
Example 3
Magnetic Fe3O4Preparing nano particles: weighing 30ml of deionized water, adding the deionized water into a 100ml beaker, weighing 1.68g of ferric chloride and 0.86g of ferrous chloride, adding the ferric chloride and the ferrous chloride into the beaker, heating the mixture at the temperature of 60 ℃, and stirring the mixture for 30 minutes to completely dissolve the ferric chloride and the ferrous chloride to obtain an orange uniform solution; adding sodium hydroxide solution to the solution, adjusting PH = 10.5; adding 0.26g trisodium citrate into the solution, heating to 80 deg.C, stirring for 60 min, stopping heating, and filtering the reaction solution to obtainFe(OH)2And Fe (OH)3Filtering the mixture; centrifugally washing the filtrate with ultrapure water for three times, and drying at 120 deg.C for 2.5 hr to obtain magnetic Fe3O4And (3) nanoparticles.
La2(MoO4)3:Eu3+Preparing fluorescent nanoparticles: weighing a proper amount of concentrated nitric acid (with the concentration of 68%) and adding the concentrated nitric acid into a 100ml beaker, weighing 0.86g of lanthanum oxide and 0.42g of europium oxide, uniformly mixing, adding the mixture into the beaker, heating the mixture to the temperature of 50 ℃, heating the mixture to 85 ℃ after the lanthanum oxide and the europium oxide are completely dissolved, and evaporating redundant concentrated nitric acid to obtain white powdery lanthanum nitrate and europium nitrate; dissolving white powdery lanthanum nitrate and europium nitrate with a proper amount of ultrapure water, adding 3.7ml of 99% polyethyleneimine solution, and uniformly mixing to form a solution A; weighing 2.81g of sodium molybdate, and dissolving with a proper amount of ultrapure water to form a solution B; under magnetic stirring, quickly injecting the solution B into the solution A to form a mixed solution; adding ammonia water into the mixed solution, adjusting the pH =10, and then continuing stirring for 12 minutes; then transferring the mixed solution into a hydrothermal reaction kettle, sealing and reacting the mixed solution at 160 ℃ for 6 hours; after the reaction kettle is cooled to room temperature, unsealing, and centrifugally separating reactants to obtain a white precipitate; washing the white precipitate with ultrapure water and absolute ethyl alcohol for three times respectively, and then putting the washed white precipitate into a constant-temperature oven at 70 ℃ for full drying to obtain La2(MoO4)3:Eu3+Fluorescent nanoparticles.
Preparing a magnetic fluorescent nano composite material: subjecting the obtained La to2(MoO4)3:Eu3+Fluorescent nanoparticles and magnetic Fe3O4The nano particles are added into a proper amount of absolute ethyl alcohol according to the proportion of 1:3, 1:2, 1:1, 1.5:1, 2:1, 2.5:1, 3:1, 4:1 and 5:1, and are blended to form the magnetic fluorescent nano composite material.
Example 4
Magnetic Fe3O4Preparing nano particles: weighing 30ml of deionized water, adding into 100ml of beaker, weighing 2.23g of ferric chloride and 1.14g of ferrous chloride, adding into the beaker, heating to 70 ℃, heating and stirring for 20 minutes to completely dissolve the ferric chloride and the ferrous chloride to obtain the orange yellowA homogeneous solution of color; adding sodium hydroxide solution to the solution, adjusting PH = 11; adding 0.3g trisodium citrate into the solution, heating to 90 deg.C, heating and stirring for 50 min, stopping heating, and filtering the reaction solution to obtain Fe (OH)2And Fe (OH)3Filtering the mixture; centrifugally washing the filtrate with ultrapure water for three times, and drying at 130 deg.C for 2 hr to obtain magnetic Fe3O4And (3) nanoparticles.
La2(MoO4)3:Eu3+Preparing fluorescent nanoparticles: weighing a proper amount of concentrated nitric acid (with the concentration of 68%) and adding the concentrated nitric acid into a 100ml beaker, weighing 1.14g of lanthanum oxide and 0.53g of europium oxide, uniformly mixing, adding the mixture into the beaker, heating the mixture to the temperature of 60 ℃, heating the mixture to the temperature of 90 ℃ after the lanthanum oxide and the europium oxide are completely dissolved, and evaporating redundant concentrated nitric acid to obtain white powdery lanthanum nitrate and europium nitrate; dissolving white powdery lanthanum nitrate and europium nitrate in a proper amount of ultrapure water, adding 5ml of 99% polyethyleneimine solution, and uniformly mixing to form a solution A; weighing 3.63g of sodium molybdate, and dissolving with a proper amount of ultrapure water to form a solution B; under magnetic stirring, quickly injecting the solution B into the solution A to form a mixed solution; adding ammonia water into the mixed solution, adjusting the pH =12, and continuing stirring for 15 minutes; then transferring the mixed solution into a hydrothermal reaction kettle, sealing and reacting the mixed solution at 170 ℃ for 5 hours; after the reaction kettle is cooled to room temperature, unsealing, and centrifugally separating reactants to obtain a white precipitate; washing the white precipitate with ultrapure water and absolute ethyl alcohol for three times respectively, and then putting the washed white precipitate into a constant-temperature oven at 80 ℃ for full drying to obtain La2(MoO4)3:Eu3+Fluorescent nanoparticles.
Preparing a magnetic fluorescent nano composite material: subjecting the obtained La to2(MoO4)3:Eu3+Fluorescent nanoparticles and magnetic Fe3O4The nanometer particles are added into a proper amount of ultrapure water according to the proportion of 1:3, 1:2, 1:1, 1.5:1, 2:1, 2.5:1, 3:1, 4:1 and 5:1, and are blended to form the magnetic fluorescent nanometer composite material.
As shown in FIG. 1, the magnetic fluorescent nanocomposite obtained in example 1 was randomly sampled to perform a luminescence coloration test (irradiation with a laser having a wavelength of 365 nm); by detecting the actual luminous performance of the magnetic fluorescent nano composite material, the nano particles can emit bright fluorescence, and the monitoring function can be realized.
As shown in fig. 2, the magnetic fluorescent nanocomposite obtained in example 2 was randomly sampled for particle size testing; the particle size of the magnetic fluorescent nanocomposite was analyzed by a laser particle sizer, and the results showed that the nanoparticles had a nano size.
As shown in fig. 3, the magnetic fluorescent nanocomposite obtained in example 3 was randomly sampled for fluorescence intensity test; the fluorescence property of the magnetic fluorescent nano composite material is characterized by a fluorescence spectrophotometer (note: two fluorescence curves positioned at the lowest parts 1:3 and 1:2 in the figure are basically coincident), the nano particles have better fluorescence intensity, and the fluorescence intensity is increased along with the increase of the proportion of the rare earth fluorescent nano particles.
As shown in FIG. 4, the magnetic fluorescent nanocomposite obtained in example 4 and pure magnetic Fe were randomly extracted3O4Carrying out a hysteresis loop comparison test on the nanoparticles; by representing a magnetic hysteresis loop of the magnetic fluorescent nano composite material, the nano particles have higher magnetism and can respond to the change of a magnetic field well.
The verification of the embodiment proves that the ferroferric oxide particles with good magnetism are prepared by ferric chloride and ferrous chloride through a coprecipitation method, then the fluorescent particles are synthesized by three rare earth ions through a hydrothermal method, the magnetic fluorescent nano particles are compounded into a whole through a blending method, and finally, through utilizing fluorescence, particle size and Vibration Sample Magnetometer (VSM) and irradiating by a laser with the wavelength of 365nm, the visible red light can be seen, the magnetic fluorescent nano particles have good magnetism, the fluorescent layer on the surface is thick, and the fluorescence luminosity is strong.
Finally, it should be noted that the above-mentioned embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same, and although the present invention is described in detail with reference to the above-mentioned embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the specific embodiments of the present invention without departing from the spirit and scope of the present invention, and all the modifications or equivalent substitutions should be covered in the claims of the present invention.
Claims (9)
1. The preparation method of the magnetic fluorescent nano composite material is characterized by comprising the following steps of:
(1) preparing magnetic nanoparticles: magnetic Fe is prepared by adopting ferric chloride and ferrous chloride through a coprecipitation method3O4A nanoparticle;
(2) preparing fluorescent nanoparticles: la is prepared by three rare earth ions through a hydrothermal method2(MoO4)3:Eu3+Fluorescent nanoparticles, wherein three rare earth ions are respectively lanthanum ions, europium ions and molybdenum ions;
(3) preparing a magnetic fluorescent nano composite material: mixing La2(MoO4)3:Eu3+Fluorescent nanoparticles and magnetic Fe3O4The nano particles are added into ultrapure water or absolute ethyl alcohol according to a certain proportion and blended to obtain the magnetic fluorescent nano composite material.
2. The method of claim 1, wherein the magnetic Fe is selected from the group consisting of Fe, and Fe3O4The preparation of the nano-particles comprises the following steps:
step one, adding ferric chloride and ferrous chloride into deionized water according to a certain proportion, heating, and stirring to completely dissolve the ferric chloride and the ferrous chloride to obtain an orange uniform solution;
adding a sodium hydroxide solution or ammonia water into the solution, and adjusting the pH value of the solution;
adding trisodium citrate into the solution, heating, continuing stirring, filtering, and centrifugally washing the filtrate for multiple times by using ultrapure water;
step four, drying the filtered substances which are washed for many times at high temperature to obtain magnetic Fe3O4And (3) nanoparticles.
3. The method of preparing a magnetic fluorescent nanocomposite material according to claim 2, wherein:
in the first step, 0.6-2.23 g of ferric chloride, 0.3-1.14 g of ferrous chloride and 30ml of deionized water are added, the heating and stirring temperature is 50-70 ℃, and the heating and stirring time is 20-40 minutes;
in the second step, the pH value of the solution is controlled to be 9-11;
in the third step, 0.2-0.3 g of trisodium citrate is added, the temperature is raised to 70-90 ℃, and the mixture is heated and stirred for 50-70 minutes;
in the fourth step, the high-temperature drying temperature is 110-130 ℃, and the high-temperature drying time is 2-3 hours.
4. The method for preparing a magnetic fluorescent nanocomposite material according to claim 1, 2 or 3, wherein: the ferric chloride can adopt ferric chloride hexahydrate, and the ferrous chloride can adopt ferrous chloride tetrahydrate.
5. The method of claim 1, wherein the La is selected from the group consisting of2(MoO4)3:Eu3+The preparation of the fluorescent nanoparticles comprises the following steps:
firstly, weighing lanthanum oxide and europium oxide according to a proportion, uniformly mixing, adding concentrated nitric acid, heating to dissolve rare earth oxide, and evaporating redundant concentrated nitric acid to dryness to obtain white powdery rare earth nitrate;
dissolving white powdery rare earth nitrate in ultrapure water, adding a polyethyleneimine solution, and uniformly mixing to form a solution A;
weighing sodium molybdate according to a proportion, dissolving the sodium molybdate with ultrapure water to form a solution B, quickly injecting the solution B into the solution A under magnetic stirring, adding ammonia water into the mixed solution, adjusting the pH value of the mixed solution, and continuing stirring;
step four, transferring the mixed solution into a hydrothermal reaction kettle, sealing the kettle, and reacting for a certain time at a certain temperatureUnsealing after the reaction kettle is cooled to room temperature, centrifugally separating reactants to obtain white precipitate, washing the white precipitate with ultrapure water and absolute ethyl alcohol for multiple times respectively, and fully drying the precipitate after multiple times of washing in a constant-temperature oven to obtain La2(MoO4)3:Eu3+Fluorescent nanoparticles.
6. The method of claim 5, wherein the magnetic fluorescent nanocomposite material comprises:
in the first step, 0.3-1.14 g of lanthanum oxide and 0.2-0.53 g of europium oxide are added, the heating and dissolving temperature is 40-60 ℃, and the evaporation temperature is 80-90 ℃;
in the second step, the concentration of the added polyethyleneimine solution is 99%, and the volume of the added polyethyleneimine solution is 1-5 ml;
in the third step, 1.21-3.63 g of sodium molybdate is added, the pH value of the mixed solution is controlled to be 8-12, and the mixture is continuously stirred for 10-15 minutes;
in the fourth step, the reaction temperature after the hydrothermal reaction kettle is sealed is 140-170 ℃, the reaction time is 5-8 hours, and the constant temperature drying temperature is 60-80 ℃.
7. The method of claim 1, wherein the magnetic fluorescent nanocomposite material comprises: when blended, the La2(MoO4)3:Eu3+Fluorescent nanoparticles and said magnetic Fe3O4The addition ratio of the nanoparticles is 1: 3-5: 1.
8. A magnetic fluorescent nanocomposite, characterized by: the preparation method of any one of claims 1 to 7.
9. Use of a magnetic fluorescent nanocomposite material, characterized in that: use of the magnetic fluorescent nanocomposite material according to claim 8 in a fault indicator in the field of electrical power detection.
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