CN104045104A - Preparation method of fluorescence-enhanced rear-earth metal oxide nanosheet sol with positive charges - Google Patents
Preparation method of fluorescence-enhanced rear-earth metal oxide nanosheet sol with positive charges Download PDFInfo
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Abstract
The invention discloses a preparation method of fluorescence-enhanced rear-earth metal oxide nanosheet sol with positive charges. The method takes yttrium oxide, europium oxide, terbium oxide, ammonium bromide, sodium benzoate, HTTA (thenoyltrifluoroacetone) and the like as materials. The preparation method comprises the steps of firstly, roasting at a high temperature to obtain Y1.93Ln0.1O3 and Y0.95Ln0.05OBr layered materials; under microwave heating condition, intercalating for the layered materials by utilizing sodium benzoate liquor to obtain intercalated materials; and finally, carrying out ultrasonic treatment onto the intercalated materials and the HTTA in a n-butyl alcohol solvent to obtain the fluorescence-enhanced rear-earth metal oxide nanosheet sol with positive charges. The preparation method disclosed by the invention is simple in preparation process and environmental friendly.
Description
Technical field
The present invention relates to chemical synthetic material technical field, the positively charged rare-earth oxide (Y that specifically a kind of fluorescence strengthens
0.95ln
0.05o
+) preparation method of nano-film sol.
Background technology
Nano luminescent material is a kind of important solid functional materials, and because it makes its advantage that has body material to compare in various application in form and qualitative all features, the appearance of nano luminescent material has promoted the development of nano electron device greatly.Rare earth ion doped nano luminescent material causes people's extensive concern in recent years.But no matter be the quantum dot of zero dimension or the nano wire of one dimension, the rare earth ion of its internal layer all can not be fully utilized.If can obtain stratiform luminescent material, obtain the nanometer sheet luminescent material of individual layer by the method such as peeling off, those the problems referred to above just can be resolved.Due to the distinctive laminate structure of lamellar compound and interlayer chemical reactivity, make its in calorifics, mechanics, optics, electricity and magnetics, absorption, conduction, separate and catalytic field has broad application prospects.Therefore the research of lamellar compound is not only had to very important learning value, and have wide practical prospect.
The rare earth ion doped nano luminescent material great majority of previous literature report are all rare-earth hydroxide nanometer sheet, and rare-earth hydroxide nanometer sheet has certain disadvantages.Such as: in rare-earth hydroxide nanometer sheet, there is a large amount of hydroxyls, and the characteristic fluorescence of some rare earth element of the phonon coupling of hydroxyl vibrations meeting absorption (such as: Eu
3+), and then can cause the luminescent properties of rare-earth hydroxide material greatly to reduce.In addition, rare-earth hydroxide nanometer sheet poor heat stability, when exceeding after certain temperature, hydroxide nano sheet just easily destroyed by dehydration and then structure.There are not the problems referred to above in rare-earth oxide nanometer sheet.Therefore, rare-earth oxide nanometer sheet, compared with rare earth metal hydroxide nanometer sheet, has application prospect widely.
Summary of the invention
The object of this invention is to provide a kind of preparation method of positively charged rare-earth oxide nano-film sol of fluorescence enhancing, the method is taking yttrium oxide, europium sesquioxide, terbium sesquioxide, brometo de amonio, Sodium Benzoate etc. as raw material, through high temperature, microwave, the condition such as ultrasonic, obtain the positively charged rare-earth oxide nano-film sol that fluorescence strengthens.In addition, due to present method gained be the nanometer sheet with positive charge, therefore can carry out well compoundly with the nanometer sheet with negative charge, this just provides raw material for preparing the various matrix materials with property.
The concrete technical scheme that realizes the object of the invention is:
A preparation method for the positively charged rare-earth oxide nano-film sol that fluorescence strengthens, the method comprises following concrete steps:
A, get rare earth oxide Y
2o
3and Ln
2o
3wherein Y:Ln=19:1, Ln=Eu/Tb, being dissolved in a certain amount of concentration is rare nitric acid of 0.5mol/L, to just dissolving completely, obtain clear solution, then adding concentration is the oxalic acid solution of 1mol/L, obtains oxalate precipitation, till no longer producing precipitation, oxalate precipitation, 700～800 DEG C of calcinings 1～3 hour, is obtained to Y
1.9ln
0.1o
3; Get Y
1.9ln
0.1o
3put into mortar, add NH
4br, by even both ground and mixed; Wherein, NH
4br and Y
1.9ln
0.1o
3the ratio of amount of substance is 4～20:1;
B, the mixture that step a is obtained are transferred in crucible, and ram-jolt, puts into retort furnace; Temperature is 350～550 DEG C of insulations 1～3 hour, is then warming up to 620～750 DEG C of insulations 1～3 hour, and to be cooled after room temperature, taking out is also 1 × 10 by concentration successively
-4the acetic acid,diluted solution of mol/L, distilled water wash, then suction filtration, dry obtain pure Y
0.95ln
0.05oBr;
C, get the Y that step b obtains
0.95ln
0.05oBr, ratio according to 1g/100ml is placed in PhCOONa solution, by mixture 80～130 DEG C of microwaves 2 minutes in microwave oven, take out with frozen water cooling, after being down to room temperature, be again placed in microwave oven 80～130 DEG C of microwaves 2 minutes, take out with frozen water coolingly, so circulate after 5 times, washing, washing with alcohol, suction filtration, 40～70 DEG C dry obtains benzoate anion and bromide anion carries out the Y after ion-exchange
0.95ln
0.05oC
6h
5cOO; Wherein, Sodium Benzoate and Y
0.95ln
0.05the ratio of OBr amount of substance is 2:1;
D, get the Y that step c obtains
0.95ln
0.05oC
6h
5cOO, is placed in propyl carbinol solvent according to the ratio of 0.5g/100ml, adds HTTA, and ultrasonic 20 minutes, then centrifugal 15 minutes of 5000r/min, got upper strata liquid, obtains the positively charged rare-earth oxide Y that fluorescence strengthens
0.95ln
0.05o
+-TTA nano-film sol; Wherein, Y
0.95ln
0.05oC
6h
5cOO and HTTA mass ratio are 50:1.
The present invention is taking rare earth oxide, brometo de amonio, Sodium Benzoate etc. as raw material, through pyroreaction, microwave intercalation, the ultrasonic condition such as peel off, obtained the positively charged rare-earth oxide nano-film sol that fluorescence strengthens.
The invention has the beneficial effects as follows:
(1) prepare the positively charged rare-earth oxide (Y that fluorescence strengthens
0.95ln
0.05o
+-TTA) nano-film sol.
(2) in intercalation process, introduce the method for microwave, greatly save preparation time.
(3) the rare-earth oxide nanometer sheet of gained has good luminescent properties, has good application prospect in luminous field.
Brief description of the drawings
Fig. 1 is the Y that the embodiment of the present invention 1 obtains
0.95eu
0.05the XRD figure of OBr material;
Fig. 2 is the Y that the embodiment of the present invention 1 obtains
0.95eu
0.05oC
6h
5the XRD figure of COO material;
Fig. 3 is the transmitting figure of the nanometer rare earth oxide film sol plated film that obtains of the embodiment of the present invention 1; In figure: a is { Y
0.95eu
0.05o
+}
nfilm; B not exclusively modifies { Y
0.95eu
0.05o
+}
n-TTA film; C is for modifying { Y completely
0.95eu
0.05o
+}
n-TTA nanometer sheet film;
Fig. 4 is the figure that excites of the nanometer rare earth oxide film sol plated film that obtains of the embodiment of the present invention 1; In figure: a is { Y
0.95eu
0.05o
+}
nfilm; B not exclusively modifies { Y
0.95eu
0.05o
+}
n-TTA film; C is for modifying { Y completely
0.95eu
0.05o
+}
n-TTA nanometer sheet film.
Embodiment
Embodiment 1
A, get 2.0005gY
2o
3and 0.1641gEu
2o
3, being dissolved in 150ml concentration is in 0.5mol/L salpeter solution, obtains clear solution, then adding 35ml concentration is 1mol/L oxalic acid solution, obtains oxalate precipitation, and oxalate precipitation is calcined 2 hours 720 DEG C time, obtains Y
1.9eu
0.1o
3.Get 1.0529gY
1.9eu
0.1o
3, add 1.7770gNH
4br, then in mortar by even both ground and mixed.
B, the mixture that above-mentioned steps is obtained are transferred in crucible, put into retort furnace after ram-jolt.Elevated Temperature Conditions is 420 DEG C of insulations 2 hours, is then warming up to 700 DEG C of insulations 2 hours, to be cooled after room temperature, and taking out sample and using the 100ml concentration preparing in advance is successively 1 × 10
-4mol/L acetic acid solution, 200ml distilled water wash sample, then suction filtration, be drying to obtain pure Y
0.95eu
0.05oBr.
C, get the Y that the upper step of 1.0000g obtains
0.95eu
0.05oBr, be placed in the PhCOONa solution that 100ml concentration is 1.5325g/100ml, mixture 80 DEG C of microwaves in microwave oven were taken out to frozen water after 2 minutes cooling, after being down to room temperature, be again placed on 80 DEG C of microwaves of microwave oven 2 minutes, cooling, so circulate 5 times, gained sample is washed with 250ml distillation successively, 20ml washing with alcohol, suction filtration, 50 DEG C dry obtains benzoate anion and bromide anion carries out the Y after ion-exchange
0.95eu
0.05oC
6h
5cOO.
D, get the Y that 0.5000g step c obtains
0.95eu
0.05oC
6h
5cOO and 0.0100gHTTA are placed in 100ml propyl carbinol solvent, and ultrasonic 20 minutes, then centrifugal 15 minutes of 5000r/min, got upper strata liquid, obtain the positively charged rare-earth oxide (Y that fluorescence strengthens
0.95eu
0.05o
+-TTA) nano-film sol.
Embodiment 2
A, get 1.0025gY
2o
3and 0.0822gEu
2o
3, be dissolved in the salpeter solution that 80ml concentration is 0.5mol/L, obtain clear solution, then adding 25ml concentration is 1mol/L oxalic acid solution, obtains oxalate precipitation, and oxalate precipitation is calcined 2 hours 750 DEG C time, obtains Y
1.9eu
0.1o
3.Get 0.5026gY
1.9eu
0.1o
3, add 1.0602gNH
4br, then in mortar by even both ground and mixed.
B, the mixture that above-mentioned steps is obtained are transferred in crucible, put into retort furnace after ram-jolt.Elevated Temperature Conditions is 450 DEG C of insulations 2 hours, is then warming up to 680 DEG C of insulations 2 hours, to be cooled after room temperature, and taking out sample and using the 80ml concentration preparing in advance is successively 1 × 10
-4mol/L acetic acid solution, 120ml distilled water wash sample, then suction filtration, be drying to obtain pure Y
0.95eu
0.05oBr.
C, get the Y that the upper step of 1.5000g obtains
0.95eu
0.05oBr, be placed in the PhCOONa solution that 150ml concentration is 1.5325g/100ml, mixture 90 DEG C of microwaves in microwave oven were taken out to frozen water after 2 minutes cooling, after being down to room temperature, be again placed in microwave oven 90 DEG C of microwaves 2 minutes, cooling, so circulate 5 times, gained sample is washed with 3000ml distillation successively, 50ml washing with alcohol, suction filtration, 60 DEG C dry obtains benzoate anion and bromide anion carries out the Y after ion-exchange
0.95eu
0.05oC
6h
5cOO.
D, get the Y that 1.0000g step c obtains
0.95eu
0.05oC
6h
5cOO and 0.0200HTTA are placed in 200ml propyl carbinol solvent, and ultrasonic 20 minutes, then centrifugal 15 minutes of 5000r/min, got upper strata liquid, obtain the positively charged rare-earth oxide (Y that fluorescence strengthens
0.95eu
0.05o
+-TTA) nano-film sol.
Embodiment 3
A, get 3.5000gY
2o
3and 0.2985gTb
2o
3, be dissolved in the salpeter solution that 220ml concentration is 0.5mol/L, obtain clear solution, then adding 60ml concentration is 1mol/L oxalic acid solution, obtains oxalate precipitation, and oxalate precipitation is calcined 3 hours 750 DEG C time, obtains Y
1.9tb
0.1o
3.Get 2.5890gY
1.9tb
0.1o
3, add 10.8912gNH
4br, then in mortar by even both ground and mixed.
B, the mixture that above-mentioned steps is obtained are transferred in crucible, put into retort furnace after ram-jolt.Elevated Temperature Conditions is 400 DEG C of insulations 2.5 hours, is then warming up to 720 DEG C of insulations 2 hours, to be cooled after room temperature, and taking out sample and using the 250ml concentration preparing in advance is successively 1 × 10
-4mol/L acetic acid solution, 500ml distilled water wash sample, then suction filtration, be drying to obtain pure Y
0.95tb
0.05oBr.
C, get the Y that the upper step of 2.0000g obtains
0.95tb
0.05oBr, be placed on the PhCOONa solution that 200ml concentration is 1.5297g/100ml, mixture 120 DEG C of microwaves in microwave oven were taken out to frozen water after 2 minutes cooling, after being down to room temperature, be again placed in microwave oven 120 DEG C of microwaves 2 minutes, cooling, so circulate 5 times, by gained sample 400ml distillation washing, 50ml washing with alcohol, suction filtration, 55 DEG C dry obtains benzoate anion and bromide anion carries out the Y after ion-exchange
0.95tb
0.05oC
6h
5cOO.
D, get the Y that 0.5000g step c obtains
0.95tb
0.05oC
6h
5cOO and 0.0100HTTA are placed in the analytically pure propyl carbinol solvent of 100ml, and ultrasonic 20 minutes, then centrifugal 15 minutes of 5000r/min, got upper strata liquid, obtain the positively charged rare-earth oxide (Y that fluorescence strengthens
0.95tb
0.05o
+-TTA) nano-film sol.
Embodiment 4
A, get 2.0010gY
2o
3and 0.1706gTb
2o
3, being dissolved in 150ml concentration is 0.5mol/L, obtains clear solution, then adding 40ml concentration is 1mol/L oxalic acid solution, obtains oxalate precipitation, and oxalate precipitation is calcined 2 hours 780 DEG C time, obtains Y
1.9tb
0.1o
3.Get 1.0031gY
1.9tb
0.1o
3, add 5.0637gNH
4br, then in mortar by even both ground and mixed.
B, the mixture that above-mentioned steps is obtained are transferred in crucible, put into retort furnace after ram-jolt.Elevated Temperature Conditions is 400 DEG C of insulations 2 hours, is then warming up to 750 DEG C of insulations 2 hours, to be cooled after room temperature, and taking out sample and using the 100ml concentration preparing in advance is successively 1 × 10
-4mol/L acetic acid solution, 200ml distilled water wash sample, then suction filtration, be drying to obtain pure Y
0.95tb
0.05oBr.
C, get the Y that the upper step of 1.5000g obtains
0.95tb
0.05oBr, be placed in the PhCOONa solution that 150ml concentration is 1.5297g/100ml, mixture 100 DEG C of microwaves in microwave oven were taken out to frozen water after 2 minutes cooling, after being down to room temperature, be again placed in microwave oven 100 DEG C of microwaves 2 minutes, cooling, so circulate 5 times, gained sample 300ml is washed, 30ml washing with alcohol, suction filtration, 60 DEG C dry obtains benzoate anion and bromide anion carries out the Y after ion-exchange
0.95tb
0.05oC
6h
5cOO.
D, get the Y that 0.5000g step c obtains
0.95tb
0.05oC
6h
5cOO and 0.0100gHTTA are placed in 100ml propyl carbinol solvent, and ultrasonic 20 minutes, then centrifugal 15 minutes of 5000r/min, got upper strata liquid, obtain the positively charged rare-earth oxide (Y that fluorescence strengthens
0.95tb
0.05o
+-TTA) nano-film sol.
Claims (1)
1. a preparation method for the positively charged rare-earth oxide nano-film sol that fluorescence strengthens, is characterized in that the method comprises following concrete steps:
A, get rare earth oxide Y
2o
3and Ln
2o
3wherein Y:Ln=19:1, Ln=Eu/Tb, being dissolved in concentration is rare nitric acid of 0.5mol/L, to just dissolving completely, obtain clear solution, then adding concentration is the oxalic acid solution of 1mol/L, till no longer producing precipitation, obtains oxalate precipitation, oxalate precipitation, 700～800 DEG C of calcinings 1～3 hour, is obtained to Y
1.9ln
0.1o
3; Get Y
1.9ln
0.1o
3put into mortar, add NH
4br, by even both ground and mixed; Wherein, NH
4br and Y
1.9ln
0.1o
3the ratio of amount of substance is 4～20:1;
B, the mixture that step a is obtained are transferred in crucible, and ram-jolt, puts into retort furnace; Temperature is 350～550 DEG C of insulations 1～3 hour, is then warming up to 620～750 DEG C of insulations 1～3 hour, and to be cooled after room temperature, taking out is also 1 × 10 by concentration successively
-4the acetic acid,diluted solution of mol/L, distilled water wash, then suction filtration, dry obtain pure Y
0.95ln
0.05oBr;
C, get the Y that step b obtains
0.95ln
0.05oBr, ratio according to 1g/100ml is placed in PhCOONa solution, by mixture 80～130 DEG C of microwaves 2 minutes in microwave oven, take out with frozen water cooling, after being down to room temperature, be again placed in microwave oven 80～130 DEG C of microwaves 2 minutes, take out with frozen water coolingly, so circulate after 5 times, washing, washing with alcohol, suction filtration, 40～70 DEG C dry obtains benzoate anion and bromide anion carries out the Y after ion-exchange
0.95ln
0.05oC
6h
5cOO; Wherein, Sodium Benzoate and Y
0.95ln
0.05the ratio of OBr amount of substance is 2:1;
D, get the Y that step c obtains
0.95ln
0.05oC
6h
5cOO, is placed in propyl carbinol solvent according to the ratio of 0.5g/100ml, adds HTTA, and ultrasonic 20 minutes, then centrifugal 15 minutes of 5000r/min, got upper strata liquid, obtains the positively charged rare-earth oxide Y that fluorescence strengthens
0.95ln
0.05o
+-TTA nano-film sol; Wherein, Y
0.95ln
0.05oC
6h
5cOO and HTTA mass ratio are 50:1.
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| CN106395881A (en) * | 2016-09-28 | 2017-02-15 | 益阳鸿源稀土有限责任公司 | Method for removing zirconium, hafnium and calcium from coarse scandium oxide or scandium-enriched products |
| CN108251102A (en) * | 2018-01-30 | 2018-07-06 | 阜阳师范学院 | HTTA modifies the preparation method of rare-earth hydroxide nanometer sheet Fluorescence Increasing material |
| CN113735885A (en) * | 2021-09-15 | 2021-12-03 | 上海时代之光照明电器检测有限公司 | Organic ligand modified rare earth oxide nanosheet composite material, preparation method, OLED (organic light emitting diode) light emitting film, OLED device and application |
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Application publication date: 20140917 |