CN106867509A - A kind of Nd3+Conversion nano crystalline substance material and preparation method thereof and water detect application on sensitization nucleocapsid - Google Patents
A kind of Nd3+Conversion nano crystalline substance material and preparation method thereof and water detect application on sensitization nucleocapsid Download PDFInfo
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Abstract
The present invention provides a kind of Nd3+Conversion nano crystalline substance material and preparation method thereof and water detect application on sensitization nucleocapsid.The Nd for being developed3+Conversion nano crystalline substance can effectively detect the water content in organic solvent on sensitization nucleocapsid.With oleic acid and octadecylene as solvent, rare earth-iron-boron is reactant to upper conversion nano crystalline substance of the invention, is prepared from by coprecipitation, and its surface is processed using HCl then.The present invention has that easy to detect, accuracy is high, good chemical stability.Products therefrom regular shape, size uniform, particle diameter distribution are narrow.The present invention is by Nd3+Sensitization combines with core shell structure design, realizes the brilliant many mode excitations of conversion nano.Nd3+Sensitization design solves the overheating effect caused by exciting light in water detection process well, it is expected to be used widely in Chemical Manufacture, biological lesion detection field.
Description
Technical field
The invention belongs to solid luminescent material field, more particularly, to a kind of Nd3+Conversion nano crystalline substance material on sensitization nucleocapsid
And preparation method thereof and water detect application.
Background technology
Water is most common a kind of material on the earth, be including including inorganic chemical, the mankind existence of all life it is important
Resource, is also the most important part of organism.In chemical field, such as oil, the production of chemical reagent, water is a kind of normal
The impurity seen；In biomedical sector, the water content of Different Organs and tissue is an important health indicator in organism.
Therefore accurately measuring for water is applied all with highly important for industrial production, scientific research, biomedical lesion detection etc.
Meaning.
In recent years, detect that solution content has proven to the effective method of a class based on fluorescence analysis.
Fluorescence probe has the advantage such as simple to operate, noncontact, real-time detection, easily prepared and receives much concern.At present, fluorescence water probe
Research be concentrated mainly on organic fluorescence molecule aspect, and such water probe cannot detect the very small situation of water content,
And organic fluorescence molecular probe there are problems that being difficult to reuse, cause.In contrast, it is rare earth ion doped
Upper conversion nano it is brilliant with chemical stability high, narrow transmitting band, big anti-stoke shift the features such as be expected to turn into detection
A kind of very promising material of application aspect.But, the upper conversion nano for water detection of most of report is brilliant in recent years, its
Excitation wavelength is respectively positioned on 980nm [ACS Appl.Mater.Interfaces., 2016,8,847-853], and the excitation wavelength is easily
Absorbed by organism and produce overheating effect, damaging cells tissue greatly hinders its application.
The content of the invention
The purpose of the present invention is directed to the deficiencies in the prior art, proposes a kind of Nd3+Conversion nano crystalline substance material on sensitization nucleocapsid.
The present invention is by introducing rare earth Nd3+And the change of upper conversion nano crystalline substance excitation wavelength is realized with reference to core shell structure design
Change the enhancing of (808nm is changed into by 980nm) and luminous intensity, using hydrone to the strong absorption of 980nm and right
The weak absorbing effect of 808nm and the Transfer of energy between rare earth ion and hydrone are water detection mechanism, obtain one kind
Effectively, stably, be able to detect that the upper conversion nano crystalline substance water probe of minor amount of water.
Nd of the present invention3+Conversion nano crystalline substance material, is the rare earth with oleic acid and octadecylene mixed solution as solvent on sensitization nucleocapsid
Chloride is reactant (Nd3+It is sensitizer, Yb3+It is energy transfer agent, Er3+It is activator, Gd3+、Y3+It is host material), lead to
Cross coprecipitation to be prepared from, its surface is processed using HCl；On the nucleocapsid conversion nano crystalline substance material 980nm,
808nm excites down the content for being capable of detecting when Water in Organic Solvents.
Upper conversion nano crystalline form looks of the invention are hexagon, and its yardstick is 15~30nm or so.
Brilliant the first composition of upper conversion nano is Yb/Er:NaGdF4@Yb/Nd:NaYF4, its center composition is Yb/Er:
NaGdF4, the nucleocapsid composition for being coated on core periphery is Yb/Nd:NaYF4。
Brilliant second composition of upper conversion nano is Yb/1Er:NaGdF4@Yb/Nd:NaYF4@NaGdF4, its center composition be
Yb/Er:NaGdF4, the nucleocapsid composition for being coated on core periphery is Yb/Nd:NaYF4, be coated on nucleocapsid periphery nucleocapsid shell composition be
NaGdF4。
The molar percentage of Yb, Er, Gd is 20% in upper conversion nano nucleus:1%:79%, upper conversion nano nucleus shell
The molar percentage of interior Yb, Nd, Y is 20%:10%:70%.
Above-mentioned Nd3+It is sensitizer, positioned at shell, i.e., the 2nd layer；Yb3+It is energy transfer agent, positioned at core, shell, i.e., the 1st, 2
Layer；Er3+It is activator, positioned at core, i.e., the 1st layer；Gd3+Be host material, positioned at core, shell, i.e., the 1st, 3 layers；Y3+It is matrix material
Material, positioned at shell, i.e., the 2nd layer.
After upper conversion core-shell nano crystalline substance of the invention is processed through HCl (1-2M, 2-5ml) and ethanol (2-5ml) mixed solution
Without oleic acid ligand, upper conversion nano crystalline substance can be dissolved in water on surface.
In the case where 980nm and 808nm are excited, upper conversion nano crystalline substance of the invention can all send bright green glow.Will be nanocrystalline
It is added in the organic solvent of different water contents, its emissive porwer will appear from change.
It is a further object to provide above-mentioned Nd3+The preparation method of conversion nano crystalline substance material on sensitization nucleocapsid.
Upper conversion nano crystalline substance (Yb/Er:NaGdF4@Yb/Nd:NaYF4) preparation method, comprise the following steps：
The preparation of step (1), upper conversion nano nucleus structure
Rare earth-iron-boron A is added in the mixed solution of oleic acid and octadecylene, fully dissolving is formed at 140-160 DEG C
Clear solution is simultaneously down to normal temperature, is subsequently adding and is dissolved with NaOH and NH4The methanol solution of F, methyl alcohol is discharged at 50 DEG C, is then heated up
To 270-290 DEG C in N2Protection lower insulation 80-100 minutes, is finally cooled to normal temperature, with ethanol and hexamethylene to reacting what is obtained
Solution is washed, and obtains required core sample, and be dispersed in hexamethylene；
Rare earth-iron-boron A includes GdCl3·6H2O,YbCl3·6H2O,ErCl3·6H2O；Preferably, Yb, Er, Gd
Molar percentage is 20%:1%:79%.
NaOH, the addition ratio of methyl alcohol are 2mmol:5-10ml, rare earth-iron-boron A and NaOH, NH4The mol ratio of F is 1:
2-2.5:3.5-4；
The preparation of step (2), upper conversion nano nucleus shell structure
Rare earth-iron-boron B is added in the mixed solution of oleic acid and octadecylene, fully dissolving is formed at 140-160 DEG C
Clear solution is simultaneously down to normal temperature, is subsequently adding step (1) core sample, and hexamethylenes are discharged at 80 DEG C and 50 DEG C are down to, and is subsequently adding
It is dissolved with NaOH and NH4The methanol solution of F, discharges at 50 DEG C to methyl alcohol, then heats to 270-290 DEG C in N2Under protection
Insulation 150-180 minutes, is finally cooled to normal temperature, and the solution that reaction is obtained is washed with ethanol and hexamethylene, obtains institute
The sample in core periphery coated core-shell for needing, that is, go up conversion nano crystalline substance sample, and be dispersed in hexamethylene；
Rare earth-iron-boron B includes YCl3·6H2O,YbCl3·6H2O,NdCl3·6H2O；Preferably, Yb, Nd, Y's rubs
Your percentage is 20%:10%:70%.
NaOH, the addition ratio of methyl alcohol are 2mmol:5-10ml, rare earth-iron-boron B and NaOH, NH4The mol ratio of F is 1:
2-2.5:3.5-4；
The brilliant post processing of step (3), upper conversion nano
The upper conversion nano crystalline substance sample that step (2) is obtained is washed with the mixed liquor of HCl and ethanol, ultrasonic, centrifugation is obtained
Final product.
Upper conversion nano crystalline substance (Yb/Er:NaGdF4@Yb/Nd:NaYF4@NaGdF4) preparation method, comprise the following steps：
The preparation of step (1), upper conversion nano nucleus structure
Rare earth-iron-boron A is added in the mixed solution of oleic acid and octadecylene, fully dissolving is formed at 140-160 DEG C
Clear solution is simultaneously down to normal temperature, is subsequently adding and is dissolved with NaOH and NH4The methanol solution of F, methyl alcohol is discharged at 50 DEG C, is then heated up
To 270-290 DEG C in N2Protection lower insulation 80-100 minutes, is finally cooled to normal temperature, with ethanol and hexamethylene to reacting what is obtained
Solution is washed, and obtains required core sample, and be dispersed in hexamethylene；
Rare earth-iron-boron A includes GdCl3·6H2O,YbCl3·6H2O,ErCl3·6H2O；Preferably, Yb, Er, Gd
Molar percentage is 20%:1%:79%.
NaOH, the addition ratio of methyl alcohol are 2mmol:5-10ml, rare earth-iron-boron A and NaOH, NH4The mol ratio of F is 1:
2-2.5:3.5-4；
The preparation of step (2), upper conversion nano nucleus shell structure
Rare earth-iron-boron B is added in the mixed solution of oleic acid and octadecylene, fully dissolving is formed at 140-160 DEG C
Clear solution is simultaneously down to normal temperature, is subsequently adding step (1) core sample, and hexamethylenes are discharged at 80 DEG C and 50 DEG C are down to, and is subsequently adding
It is dissolved with NaOH and NH4The methanol solution of F, discharges at 50 DEG C to methyl alcohol, then heats to 270-290 DEG C in N2Under protection
Insulation 150-180 minutes, is finally cooled to normal temperature, and the solution that reaction is obtained is washed with ethanol and hexamethylene, obtains institute
The sample in core periphery coated core-shell for needing, and be dispersed in hexamethylene；
Rare earth-iron-boron B includes YCl3·6H2O,YbCl3·6H2O,NdCl3·6H2O；Preferably, Yb, Nd, Y's rubs
Your percentage is 20%:10%:70%.
NaOH, the addition ratio of methyl alcohol are 2mmol:5-10ml, rare earth-iron-boron B and NaOH, NH4The mol ratio of F is 1:
2-2.5:3.5-4；
The preparation of step (3), upper conversion nano nucleus shell shell structure
Rare earth-iron-boron C is added in the mixed solution of oleic acid and octadecylene, fully dissolving is formed at 140-160 DEG C
Clear solution is simultaneously down to normal temperature, is subsequently adding sample of the step (2) in core periphery coated core-shell, hexamethylene is discharged at 80 DEG C and is dropped
To 50 DEG C, it is subsequently adding and is dissolved with NaOH and NH4The methanol solution of F, methyl alcohol is discharged at 50 DEG C, then heats to 270-290 DEG C
In N2Protection lower insulation 150-180 minutes, is finally cooled to normal temperature, and the solution that reaction is obtained is washed with ethanol and hexamethylene
Wash, obtain the required sample in nucleocapsid periphery coated core-shell shell, that is, go up conversion nano crystalline substance sample, and be dispersed in hexamethylene；
Rare earth-iron-boron C includes GdCl3·6H2O；
NaOH, the addition ratio of methyl alcohol are 2mmol:5-10ml, rare earth-iron-boron C and NaOH, NH4The mol ratio of F is 1:
2-2.5:3.5-4；
The brilliant post processing of step (4), upper conversion nano
The upper conversion nano crystalline substance sample that step (3) is obtained is washed with the mixed liquor of HCl and ethanol, ultrasonic, centrifugation is obtained
Final product.
Preferably, step (1) rare earth-iron-boron A is 0.8-1mmol with the addition ratio of oleic acid, octadecylene：8ml：
12ml；
Preferably, step (2) rare earth-iron-boron B is 0.8-1mmol with the addition ratio of oleic acid, octadecylene：8ml：
12ml；
Preferably, step (3) rare earth-iron-boron C is 0.8-1mmol with the addition ratio of oleic acid, octadecylene：8ml：
12ml。
Transmission electron microscope observation shows synthesized upper conversion nano crystalline form looks for hexagon, its yardstick is 20~
30nm or so.Fourier's INFRARED SPECTRUM shows to match somebody with somebody without oleic acid through the upper conversion nano crystalline substance surface after HCl, alcohol mixed solution treatment
Body.In the case where 980nm and 808nm are excited, upper conversion nano crystalline substance can send bright green glow, and its transmitting band centre wavelength is located at
540nm and 654nm.
A further object of the present invention is to provide above-mentioned Nd3+Conversion nano crystalline substance material is used as water detection probe on sensitization nucleocapsid
Application.
The upper conversion nano of above-mentioned acquisition is brilliant to utilize strong absorption of the hydrone to 980nm and the weak suction to 808nm
Transfer of energy between adduction and rare earth ion and hydrone can realize the water in organic solvent for water detection mechanism
Content detection.
The present invention has that easy to detect, accuracy is high, good chemical stability.Products therefrom regular shape, size
Uniformly, particle diameter distribution is narrow.The present invention is by Nd3+Sensitization combines with core shell structure design, realizes many of conversion nano crystalline substance
Mode excitation.Nd3+Sensitization design solves the overheating effect caused by exciting light in water detection process well, it is expected in chemical industry life
Produce, biological lesion detection field is used widely.In the case where 980nm and 808nm are excited, the upper conversion nano of different core shell structures
Brilliant water Detection results are different, and this provides various Sexual behavior mode for us in the detection application of actual water.
Nd of the present invention3+Conversion nano crystalline substance water probe has good water detection performance on sensitization nucleocapsid, in organic solvent
The detectable limit of water content can reach 100ppm.
Brief description of the drawings
Fig. 1 is the transmission electron microscope picture of conversion nano nucleus on nucleocapsid shell in example 1；
Fig. 2 is the brilliant transmission electron microscope picture of conversion nano on nucleocapsid in example 2；
Fig. 3 is the transmission electron microscope picture of upper conversion nano nucleus in comparative example 3；
Fig. 4 is the brilliant high-resolution-ration transmission electric-lens figure of conversion nano on nucleocapsid in example 2；
Fig. 5 is the brilliant high angle annular dark field scanning transmission electron microscope figure of conversion nano on nucleocapsid shell in example 1；
Fig. 6 is the brilliant high angle annular dark field scanning transmission electron microscope figure of conversion nano on nucleocapsid in example 2；
Fig. 7 is that upper conversion nano nucleus is infrared by the Fourier after HCl, alcohol mixed solution before processing in comparative example 3
Spectrum；
Fig. 8 is the transmitting under nucleocapsid shell in example 1,2,3, nucleocapsid, the upper conversion nano crystalline substance of nuclear structure are excited at 980 nanometers
Spectrum；
Fig. 9 is that nucleocapsid shell in example 1,2,3, nucleocapsid, the upper conversion nano crystalline substance of nuclear structure excite lower emission spectra at 980 nanometers
540 nanometers of fluorescence lifetime；
Figure 10 is that nucleocapsid shell in example 1,2,3, nucleocapsid, the upper conversion nano crystalline substance of nuclear structure excite lower transmitting at 980 nanometers
The fluorescence lifetime of 654 nanometers of spectrum；
Figure 11 is the emission spectra under nucleocapsid shell in example 1,2, the upper conversion nano crystalline substance of core shell structure are excited at 808 nanometers；
Figure 12 is that nucleocapsid shell in example 1,2, the upper conversion nano crystalline substance of core shell structure excite lower emission spectra 540 at 808 nanometers
The fluorescence lifetime of nanometer；
Figure 13 is that nucleocapsid shell in example 1,2, the upper conversion nano crystalline substance of core shell structure excite lower emission spectra 654 at 808 nanometers
The fluorescence lifetime of nanometer；
Figure 14 is when detecting different water content solvents under conversion nano crystalline substance is excited at 808 nanometers on nucleocapsid shell in example 1
Emission spectra and luminous photo；
Under Figure 15 is nucleocapsid shell in example 1,2, conversion nano crystalline substance is excited at 808 nanometers on nucleocapsid, relative emission intensity with
The matched curve of water content change；
Specific embodiment
The present invention is further analyzed with reference to specific embodiment.
Example 1：Yb/Er (20/1mol%):NaGdF4@Yb/Nd (20/10mol%):NaYF4@NaGdF4Turn on nucleocapsid shell
Change nanocrystalline：
By rare earth-iron-boron, (integral molar quantity is 0.8mmol, wherein GdCl3·6H2O(0.632mmol),YbCl3·6H2O
(0.16mmol),ErCl3·6H2O (0.008mmol)) it is added in the mixed solution of oleic acid (8ml) and octadecylene (12ml),
Fully dissolving forms clear solution and is down to room temperature at 150 DEG C, is subsequently adding and is dissolved with NaOH (2mmol) and NH4F(3mmol)
Methanol solution (5ml), methyl alcohol is discharged at 50 DEG C, then heat to 280 DEG C in N2The lower insulation of protection 90 minutes, finally
Room temperature is cooled to, the solution that reaction is obtained is washed with ethanol and hexamethylene, obtain required core sample (Yb/Er (20/
1mol%):NaGdF4), and be dispersed in hexamethylene (3ml)；
By rare earth-iron-boron, (integral molar quantity is 0.8mmol, YCl3·6H2O(0.56mmol),YbCl3·6H2O
(0.16mmol)and NdCl3·6H2O (0.08mmol)) it is added in the mixed solution of oleic acid (8ml) and octadecylene (12ml),
Fully dissolving forms clear solution and is down to room temperature at 150 DEG C, is subsequently adding core sample (3ml, Yb/Er (20/1mol%):
NaGdF4), hexamethylenes are discharged at 80 DEG C and 50 DEG C are down to, it is subsequently adding and is dissolved with NaOH (2mmol) and NH4The first of F (3mmol)
Alcoholic solution (5ml), discharges at 50 DEG C to methyl alcohol, then heats to 280 DEG C in N2The lower insulation of protection 150 minutes, it is last cold
But room temperature is arrived, the solution that reaction is obtained is washed with ethanol and hexamethylene, obtain required nucleocapsid sample (Yb/Er (20/
1mol%):NaGdF4@Yb/Nd (20/10mol%):NaYF4), and be dispersed in hexamethylene (3ml)；
By rare earth-iron-boron (GdCl3·6H2O (0.8mmol)) it is added to the mixing of oleic acid (8ml) and octadecylene (12ml)
In solution, fully dissolving forms clear solution and is down to room temperature at 150 DEG C, is subsequently adding nucleocapsid sample (3ml, Yb/Er (20/
1mol%):NaGdF4@Yb/Nd (20/10mol%):NaYF4), hexamethylenes are discharged at 80 DEG C and 50 DEG C are down to, it is subsequently adding molten
Solution has NaOH (2mmol) and NH4The methanol solution (5ml) of F (3mmol), discharges at 50 DEG C to methyl alcohol, then heats to
280 DEG C in N2The lower insulation of protection 150 minutes, is finally cooled to room temperature, and the solution that reaction is obtained is carried out with ethanol and hexamethylene
Washing, obtains required nucleocapsid shell sample (Yb/Er (20/1mol%):NaGdF4@Yb/Nd (20/10mol%):NaYF4@
NaGdF4), and be dispersed in hexamethylene (3ml)；
The brilliant mixed liquor with HCl (1M, 2ml) and ethanol (2ml) of conversion nano on the nucleocapsid shell of above-mentioned acquisition is washed, is surpassed
Sound, centrifugation obtain final product.
Transmission electron microscope observation shows that conversion nano crystalline substance is six sides of 25-30 rans on synthesized nucleocapsid shell
Shape particle (Fig. 1).On nucleocapsid shell conversion nano crystalline substance excited at 980 nanometers and 808 nanometers it is lower can send bright green glow, pass through
The increase of shell, luminosity is strengthened (Fig. 8,11), fluorescence lifetime increase (Fig. 9,10,12,13).At 980 nanometers and
808 nanometers excite down, strong absorption using hydrone to 980nm and the effect of the weak absorbing to 808nm and rare earth from
Energy transfer between son and hydrone, the water detection on the nucleocapsid shell for being obtained in the brilliant achievable organic solvent of conversion nano.
Under being excited at 808 nanometers, conversion nano is brilliant when different water content solvents are detected on nucleocapsid shell, and the intensity of its emission spectra is with water
The increase of content and reduce (Figure 14,15).It is brilliant for conversion nano on nucleocapsid shell, under being excited at 808 nanometers, its water content compared with
Interval detection sensitivity high is (Figure 15) high.
Example 2：Yb/Er (20/1mol%):NaGdF4@Yb/Nd (20/10mol%):NaYF4Conversion nano is brilliant on nucleocapsid：
By rare earth-iron-boron, (integral molar quantity is 0.8mmol, wherein GdCl3·6H2O(0.632mmol),YbCl3·6H2O
(0.16mmol),ErCl3·6H2O (0.008mmol)) it is added in the mixed solution of oleic acid (8ml) and octadecylene (12ml),
Fully dissolving forms clear solution and is down to room temperature at 150 DEG C, is subsequently adding and is dissolved with NaOH (2mmol) and NH4F(3mmol)
Methanol solution (5ml), methyl alcohol is discharged at 50 DEG C, then heat to 280 DEG C in N2The lower insulation of protection 90 minutes, finally
Room temperature is cooled to, the solution that reaction is obtained is washed with ethanol and hexamethylene, obtain required core sample (Yb/Er (20/
1mol%):NaGdF4), and be dispersed in hexamethylene (3ml)；
By rare earth-iron-boron, (integral molar quantity is 0.8mmol, YCl3·6H2O(0.56mmol),YbCl3·6H2O
(0.16mmol)and NdCl3·6H2O (0.08mmol)) it is added in the mixed solution of oleic acid (8ml) and octadecylene (12ml),
Fully dissolving forms clear solution and is down to room temperature at 150 DEG C, is subsequently adding core sample (3ml, Yb/Er (20/1mol%):
NaGdF4), hexamethylenes are discharged at 80 DEG C and 50 DEG C are down to, it is subsequently adding and is dissolved with NaOH (2mmol) and NH4The first of F (3mmol)
Alcoholic solution (5ml), discharges at 50 DEG C to methyl alcohol, then heats to 280 DEG C in N2The lower insulation of protection 150 minutes, it is last cold
But room temperature is arrived, the solution that reaction is obtained is washed with ethanol and hexamethylene, obtain required nucleocapsid sample (Yb/Er (20/
1mol%):NaGdF4@Yb/Nd (20/10mol%):NaYF4), and be dispersed in hexamethylene (3ml)；
The brilliant mixed liquor with HCl (1M, 2ml) and ethanol (2ml) of conversion nano on the nucleocapsid of above-mentioned acquisition is washed, is surpassed
Sound, centrifugation obtain final product.
Transmission electron microscope observation shows that conversion nano crystalline substance is the hexagon of 30 rans on synthesized nucleocapsid
Grain (Fig. 2).Conversion nano crystalline substance is excited at 980 nanometers and 808 nanometers and lower can send brighter green glow (Fig. 8,11) on nucleocapsid.
980 nanometers and 808 nanometers excite down, strong absorption using hydrone to 980nm and the effect of the weak absorbing to 808nm with
And the energy transfer between rare earth ion and hydrone, the water on the nucleocapsid for being obtained in the brilliant achievable organic solvent of conversion nano
Detection.Brilliant for conversion nano on nucleocapsid, under being excited at 808 nanometers, it is in the relatively low interval detection sensitivity (figure high of water content
15)。
Example 3：Yb/Er (20/1mol%):NaGdF4@Yb/Nd (20/10mol%):NaYF4@NaGdF4Turn on nucleocapsid shell
Change nanocrystalline：
By rare earth-iron-boron, (integral molar quantity is 1mmol, wherein GdCl3·6H2O(0.79mmol),YbCl3·6H2O
(0.2mmol),ErCl3·6H2O (0.01mmol)) it is added in the mixed solution of oleic acid (8ml) and octadecylene (12ml),
Fully dissolving forms clear solution and is down to room temperature at 140 DEG C, is subsequently adding and is dissolved with NaOH (2mmol) and NH4F(3mmol)
Methanol solution (10ml), methyl alcohol is discharged at 50 DEG C, then heat to 270 DEG C in N2The lower insulation of protection 100 minutes, most
After be cooled to room temperature, the solution that reaction is obtained is washed with ethanol and hexamethylene, obtain required core sample (Yb/Er
(20/1mol%):NaGdF4), and be dispersed in hexamethylene (6ml)；
By rare earth-iron-boron, (integral molar quantity is 1mmol, YCl3·6H2O(0.7mmol),YbCl3·6H2O(0.2mmol)
and NdCl3·6H2O (0.1mmol)) it is added in the mixed solution of oleic acid (8ml) and octadecylene (12ml), filled at 140 DEG C
Divide dissolving to form clear solution and be down to room temperature, be subsequently adding core sample (3ml, Yb/Er (20/1mol%):NaGdF4), 80
DEG C discharge hexamethylene is simultaneously down to 50 DEG C, is subsequently adding and is dissolved with NaOH (2mmol) and NH4The methanol solution (5ml) of F (3mmol),
Methyl alcohol is discharged at 50 DEG C, then heats to 270 DEG C in N2The lower insulation of protection 180 minutes, is finally cooled to room temperature, uses second
Alcohol and hexamethylene are washed to the solution that reaction is obtained, and obtain required nucleocapsid sample (Yb/Er (20/1mol%):
NaGdF4@Yb/Nd (20/10mol%):NaYF4), and be dispersed in hexamethylene (6ml)；
By rare earth-iron-boron (GdCl3·6H2O (0.8mmol)) it is added to the mixing of oleic acid (8ml) and octadecylene (12ml)
In solution, fully dissolving forms clear solution and is down to room temperature at 150 DEG C, is subsequently adding nucleocapsid sample (3ml, Yb/Er (20/
1mol%):NaGdF4@Yb/Nd (20/10mol%):NaYF4), hexamethylenes are discharged at 80 DEG C and 50 DEG C are down to, it is subsequently adding molten
Solution has NaOH (2mmol) and NH4The methanol solution (5ml) of F (3mmol), discharges at 50 DEG C to methyl alcohol, then heats to
270 DEG C in N2The lower insulation of protection 180 minutes, is finally cooled to room temperature, and the solution that reaction is obtained is carried out with ethanol and hexamethylene
Washing, obtains required nucleocapsid shell sample (Yb/Er (20/1mol%):NaGdF4@Yb/Nd (20/10mol%):NaYF4@
NaGdF4), and be dispersed in hexamethylene (3ml)；
The brilliant mixed liquor with HCl (1M, 2ml) and ethanol (2ml) of conversion nano on the nucleocapsid shell of above-mentioned acquisition is washed, is surpassed
Sound, centrifugation obtain final product.
Example 4：Yb/Er (20/1mol%):NaGdF4@Yb/Nd (20/10mol%):NaYF4@NaGdF4Turn on nucleocapsid shell
Change nanocrystalline：
By rare earth-iron-boron, (integral molar quantity is 1mmol, wherein GdCl3·6H2O(0.79mmol),YbCl3·6H2O
(0.2mmol),ErCl3·6H2O (0.01mmol)) it is added in the mixed solution of oleic acid (8ml) and octadecylene (12ml),
Fully dissolving forms clear solution and is down to room temperature at 160 DEG C, is subsequently adding and is dissolved with NaOH (2.5mmol) and NH4F
The methanol solution (12.5ml) of (3.75mmol), discharges at 50 DEG C to methyl alcohol, then heats to 290 DEG C in N2Protection is lower to be protected
Temperature 80 minutes, is finally cooled to room temperature, and the solution that reaction is obtained is washed with ethanol and hexamethylene, obtains required core sample
Product (Yb/Er (20/1mol%):NaGdF4), and be dispersed in hexamethylene (6ml)；
By rare earth-iron-boron, (integral molar quantity is 0.8mmol, YCl3·6H2O(0.56mmol),YbCl3·6H2O
(0.16mmol)and NdCl3·6H2O (0.08mmol)) it is added in the mixed solution of oleic acid (8ml) and octadecylene (12ml),
Fully dissolving forms clear solution and is down to room temperature at 160 DEG C, is subsequently adding core sample (3ml, Yb/Er (20/1mol%):
NaGdF4), hexamethylenes are discharged at 80 DEG C and 50 DEG C are down to, it is subsequently adding and is dissolved with NaOH (2mmol) and NH4The first of F (3mmol)
Alcoholic solution (5ml), discharges at 50 DEG C to methyl alcohol, then heats to 290 DEG C in N2The lower insulation of protection 150 minutes, it is last cold
But room temperature is arrived, the solution that reaction is obtained is washed with ethanol and hexamethylene, obtain required nucleocapsid sample (Yb/Er (20/
1mol%):NaGdF4@Yb/Nd (20/10mol%):NaYF4), and be dispersed in hexamethylene (6ml)；
By rare earth-iron-boron (GdCl3·6H2O (0.8mmol)) it is added to the mixing of oleic acid (8ml) and octadecylene (12ml)
In solution, fully dissolving forms clear solution and is down to room temperature at 150 DEG C, is subsequently adding nucleocapsid sample (3ml, Yb/Er (20/
1mol%):NaGdF4@Yb/Nd (20/10mol%):NaYF4), hexamethylenes are discharged at 80 DEG C and 50 DEG C are down to, it is subsequently adding molten
Solution has NaOH (2mmol) and NH4The methanol solution (5ml) of F (3mmol), discharges at 50 DEG C to methyl alcohol, then heats to
290 DEG C in N2The lower insulation of protection 150 minutes, is finally cooled to room temperature, and the solution that reaction is obtained is carried out with ethanol and hexamethylene
Washing, obtains required nucleocapsid shell sample (Yb/Er (20/1mol%):NaGdF4@Yb/Nd (20/10mol%):NaYF4@
NaGdF4), and be dispersed in hexamethylene (6ml)；
The brilliant mixed liquor with HCl (1M, 2ml) and ethanol (2ml) of conversion nano on the nucleocapsid shell of above-mentioned acquisition is washed, is surpassed
Sound, centrifugation obtain final product.
Example 5：Yb/Er (20/1mol%):NaGdF4@Yb/Nd (20/10mol%):NaYF4@NaGdF4Turn on nucleocapsid shell
Change nanocrystalline：
By rare earth-iron-boron, (integral molar quantity is 1mmol, wherein GdCl3·6H2O(0.79mmol),YbCl3·6H2O
(0.2mmol),ErCl3·6H2O (0.01mmol)) it is added in the mixed solution of oleic acid (8ml) and octadecylene (12ml),
Fully dissolving forms clear solution and is down to room temperature at 140 DEG C, is subsequently adding and is dissolved with NaOH (2mmol) and NH4F(3mmol)
Methanol solution (10ml), methyl alcohol is discharged at 50 DEG C, then heat to 270 DEG C in N2The lower insulation of protection 100 minutes, most
After be cooled to room temperature, the solution that reaction is obtained is washed with ethanol and hexamethylene, obtain required core sample (Yb/Er
(20/1mol%):NaGdF4), and be dispersed in hexamethylene (6ml)；
By rare earth-iron-boron, (integral molar quantity is 1mmol, YCl3·6H2O(0.7mmol),YbCl3·6H2O(0.2mmol)
and NdCl3·6H2O (0.1mmol)) it is added in the mixed solution of oleic acid (8ml) and octadecylene (12ml), filled at 140 DEG C
Divide dissolving to form clear solution and be down to room temperature, be subsequently adding core sample (3ml, Yb/Er (20/1mol%):NaGdF4), 80
DEG C discharge hexamethylene is simultaneously down to 50 DEG C, is subsequently adding and is dissolved with NaOH (2mmol) and NH4The methanol solution (5ml) of F (3mmol),
Methyl alcohol is discharged at 50 DEG C, then heats to 270 DEG C in N2The lower insulation of protection 180 minutes, is finally cooled to room temperature, uses second
Alcohol and hexamethylene are washed to the solution that reaction is obtained, and obtain required nucleocapsid sample (Yb/Er (20/1mol%):
NaGdF4@Yb/Nd (20/10mol%):NaYF4), and be dispersed in hexamethylene (6ml)；
The brilliant mixed liquor with HCl (1M, 2ml) and ethanol (2ml) of conversion nano on the nucleocapsid of above-mentioned acquisition is washed, is surpassed
Sound, centrifugation obtain final product.
Example 6：Yb/Er (20/1mol%):NaGdF4@Yb/Nd (20/10mol%):NaYF4@NaGdF4Turn on nucleocapsid shell
Change nanocrystalline：
By rare earth-iron-boron, (integral molar quantity is 1mmol, wherein GdCl3·6H2O(0.79mmol),YbCl3·6H2O
(0.2mmol),ErCl3·6H2O (0.01mmol)) it is added in the mixed solution of oleic acid (8ml) and octadecylene (12ml),
Fully dissolving forms clear solution and is down to room temperature at 160 DEG C, is subsequently adding and is dissolved with NaOH (2mmol) and NH4F(3mmol)
Methanol solution (10ml), methyl alcohol is discharged at 50 DEG C, then heat to 290 DEG C in N2The lower insulation of protection 80 minutes, most
After be cooled to room temperature, the solution that reaction is obtained is washed with ethanol and hexamethylene, obtain required core sample (Yb/Er
(20/1mol%):NaGdF4), and be dispersed in hexamethylene (6ml)；
By rare earth-iron-boron, (integral molar quantity is 0.8mmol, YCl3·6H2O(0.56mmol),YbCl3·6H2O
(0.16mmol)and NdCl3·6H2O (0.08mmol)) it is added in the mixed solution of oleic acid (8ml) and octadecylene (12ml),
Fully dissolving forms clear solution and is down to room temperature at 160 DEG C, is subsequently adding core sample (3ml, Yb/Er (20/1mol%):
NaGdF4), hexamethylenes are discharged at 80 DEG C and 50 DEG C are down to, it is subsequently adding and is dissolved with NaOH (2mmol) and NH4The first of F (3mmol)
Alcoholic solution (5ml), discharges at 50 DEG C to methyl alcohol, then heats to 290 DEG C in N2The lower insulation of protection 150 minutes, it is last cold
But room temperature is arrived, the solution that reaction is obtained is washed with ethanol and hexamethylene, obtain required nucleocapsid sample (Yb/Er (20/
1mol%):NaGdF4@Yb/Nd (20/10mol%):NaYF4), and be dispersed in hexamethylene (6ml)；
The brilliant mixed liquor with HCl (1M, 2ml) and ethanol (2ml) of conversion nano on the nucleocapsid of above-mentioned acquisition is washed, is surpassed
Sound, centrifugation obtain final product.
Comparative example 1：Yb/Er (20/1mol%):NaGdF4Upper conversion nano nucleus：
By rare earth-iron-boron, (integral molar quantity is 0.8mmol, wherein GdCl3·6H2O(0.632mmol),YbCl3·6H2O
(0.16mmol),ErCl3·6H2O (0.008mmol)) it is added in the mixed solution of oleic acid (8ml) and octadecylene (12ml),
Fully dissolving forms clear solution and is down to room temperature at 150 DEG C, is subsequently adding and is dissolved with NaOH (2mmol) and NH4F(3mmol)
Methanol solution (5ml), methyl alcohol is discharged at 50 DEG C, then heat to 280 DEG C in N2The lower insulation of protection 90 minutes, finally
Room temperature is cooled to, the solution that reaction is obtained is washed with ethanol and hexamethylene, obtain required core sample (Yb/Er (20/
1mol%):NaGdF4), and be dispersed in hexamethylene (3ml)；
The upper conversion nano nucleus of above-mentioned acquisition is washed with the mixed liquor of HCl (1M, 2ml) and ethanol (2ml), ultrasound,
Centrifugation obtains final product.
Transmission electron microscope observation shows the hexagon particle that synthesized upper conversion nano nucleus is 15 rans
(Fig. 3).Brilliant compared to conversion nano on nucleocapsid, nucleocapsid shell, the emissive porwer of core is most weak (Fig. 8,11).Upper conversion nano nucleus passes through
After HCl, alcohol mixed solution treatment, the oleic acid ligand on its surface is removed (Fig. 7).
Above-described embodiment is not that, for limitation of the invention, the present invention is not limited only to above-described embodiment, as long as meeting
Application claims, belong to protection scope of the present invention.
Claims (10)
1. a kind of Nd3+Conversion nano crystalline substance material on sensitization nucleocapsid, 980nm and 808nm is excited down can send bright green glow, and it is special
Levy is that the brilliant composition of upper conversion nano is Yb/Er:NaGdF4@Yb/Nd:NaYF4, its center composition is Yb/Er:NaGdF4, cladding
Nucleocapsid composition in core periphery is Yb/Nd:NaYF4。
2. a kind of Nd3+Conversion nano crystalline substance material on sensitization nucleocapsid, it is characterised in that the upper brilliant composition of conversion nano is Yb/Er:
NaGdF4@Yb/Nd:NaYF4@NaGdF4, its center composition is Yb/Er:NaGdF4, the nucleocapsid composition for being coated on core periphery is Yb/
Nd:NaYF4, the nucleocapsid shell composition for being coated on nucleocapsid periphery is NaGdF4。
3. a kind of Nd as claimed in claim 1 or 23+Conversion nano crystalline substance material on sensitization nucleocapsid, it is characterised in that upper conversion is received
Rice crystalline form looks are hexagon, and its yardstick is 15~30nm.
4. a kind of Nd as claimed in claim 13+The preparation method of conversion nano crystalline substance material on sensitization nucleocapsid, it is characterised in that should
Method is comprised the following steps：
The preparation of step (1), upper conversion nano nucleus structure
Rare earth-iron-boron A is added in the mixed solution of oleic acid and octadecylene, fully dissolving forms transparent at 140-160 DEG C
Solution is simultaneously down to normal temperature, is subsequently adding and is dissolved with NaOH and NH4The methanol solution of F, methyl alcohol is discharged at 50 DEG C, is then heated to
270-290 DEG C in N2Protection lower insulation 80-100 minute, is finally cooled to normal temperature, with ethanol and hexamethylene to reacting obtain molten
Liquid is washed, and obtains required core sample, and be dispersed in hexamethylene；
Rare earth-iron-boron A includes GdCl3·6H2O,YbCl3·6H2O,ErCl3·6H2O；
Rare earth-iron-boron A and NaOH, NH4The mol ratio of F is 1:2-2.5:3.5-4；
The preparation of step (2), upper conversion nano nucleus shell structure
Rare earth-iron-boron B is added in the mixed solution of oleic acid and octadecylene, fully dissolving forms transparent at 140-160 DEG C
Solution is simultaneously down to normal temperature, is subsequently adding step (1) core sample, and hexamethylenes are discharged at 80 DEG C and 50 DEG C are down to, and is subsequently adding dissolving
There is NaOH and NH4The methanol solution of F, discharges at 50 DEG C to methyl alcohol, then heats to 270-290 DEG C in N2The lower insulation of protection
150-180 minutes, normal temperature is finally cooled to, the solution that reaction is obtained is washed with ethanol and hexamethylene, needed for obtaining
Nucleocapsid sample, and be dispersed in hexamethylene；
Rare earth-iron-boron B includes YCl3·6H2O,YbCl3·6H2O,NdCl3·6H2O；
Rare earth-iron-boron B and NaOH, NH4The mol ratio of F is 1:2-2.5:3.5-4；
The brilliant post processing of step (3), upper conversion nano
Conversion nano crystalline substance sample is washed with the mixed liquor of HCl and ethanol on the nucleocapsid that step (2) is obtained, ultrasonic, centrifugation is obtained
Final product.
5. a kind of Nd as claimed in claim 23+The preparation method of conversion nano crystalline substance material on sensitization nucleocapsid, it is characterised in that should
Method is comprised the following steps：
The preparation of step (1), upper conversion nano nucleus structure
Rare earth-iron-boron A is added in the mixed solution of oleic acid and octadecylene, fully dissolving forms transparent at 140-160 DEG C
Solution is simultaneously down to normal temperature, is subsequently adding and is dissolved with NaOH and NH4The methanol solution of F, methyl alcohol is discharged at 50 DEG C, is then heated to
270-290 DEG C in N2Protection lower insulation 80-100 minute, is finally cooled to normal temperature, with ethanol and hexamethylene to reacting obtain molten
Liquid is washed, and obtains required core sample, and be dispersed in hexamethylene；
Rare earth-iron-boron A includes GdCl3·6H2O,YbCl3·6H2O,ErCl3·6H2O；
Rare earth-iron-boron A and NaOH, NH4The mol ratio of F is 1:2-2.5:3.5-4；
The preparation of step (2), upper conversion nano nucleus shell structure
Rare earth-iron-boron B is added in the mixed solution of oleic acid and octadecylene, fully dissolving forms transparent at 140-160 DEG C
Solution is simultaneously down to normal temperature, is subsequently adding step (1) core sample, and hexamethylenes are discharged at 80 DEG C and 50 DEG C are down to, and is subsequently adding dissolving
There is NaOH and NH4The methanol solution of F, discharges at 50 DEG C to methyl alcohol, then heats to 270-290 DEG C in N2The lower insulation of protection
150-180 minutes, normal temperature is finally cooled to, the solution that reaction is obtained is washed with ethanol and hexamethylene, needed for obtaining
Nucleocapsid sample, and be dispersed in hexamethylene；
Rare earth-iron-boron B includes YCl3·6H2O,YbCl3·6H2O,NdCl3·6H2O；
Rare earth-iron-boron B and NaOH, NH4The mol ratio of F is 1:2-2.5:3.5-4；
The preparation of step (3), upper conversion nano nucleus shell shell structure
Rare earth-iron-boron C is added in the mixed solution of oleic acid and octadecylene, fully dissolving forms transparent at 140-160 DEG C
Solution is simultaneously down to normal temperature, is subsequently adding step (2) nucleocapsid sample, and hexamethylenes are discharged at 80 DEG C and 50 DEG C are down to, and is subsequently adding molten
Solution has NaOH and NH4The methanol solution of F, methyl alcohol is discharged at 50 DEG C, then heats to 270-290 DEG C in N2The lower insulation 150- of protection
180 minutes, normal temperature is finally cooled to, the solution that reaction is obtained is washed with ethanol and hexamethylene, obtain required nucleocapsid
Shell sample, and be dispersed in hexamethylene；
Rare earth-iron-boron C includes GdCl3·6H2O；
Rare earth-iron-boron C and NaOH, NH4The mol ratio of F is 1:2-2.5:3.5-4；
The brilliant post processing of step (4), upper conversion nano
Conversion nano crystalline substance sample is washed with the mixed liquor of HCl and ethanol on the nucleocapsid that step (3) is obtained, ultrasonic, centrifugation is obtained
Final product.
6. a kind of Nd as described in claim 4 or 53+The preparation method of conversion nano crystalline substance material on sensitization nucleocapsid, its feature exists
In the addition ratio of step (1) rare earth-iron-boron A and oleic acid, octadecylene be 0.8-1mmol：8ml：12ml.
7. a kind of Nd as described in claim 4 or 53+The preparation method of conversion nano crystalline substance material on sensitization nucleocapsid, its feature exists
In the addition ratio of step (2) rare earth-iron-boron B and oleic acid, octadecylene be 0.8-1mmol：8ml：12ml.
8. a kind of Nd as claimed in claim 53+The preparation method of conversion nano crystalline substance material on sensitization nucleocapsid, it is characterised in that step
Suddenly (3) rare earth-iron-boron C and the addition ratio of oleic acid, octadecylene are 0.8-1mmol：8ml：12ml.
9. a kind of Nd as claimed in claim 1 or 23+Conversion nano crystalline substance material on sensitization nucleocapsid, it is characterised in that upper conversion is received
The molar percentage of Yb, Er, Gd is 20% in meter Jing He:1%:79%, moles the hundred of Yb, Nd, Y in upper conversion nano nucleus shell
Divide than being 20%:10%:70%.
10. a kind of Nd as claimed in claim 1 or 23+Conversion nano crystalline substance material is on as water detection probe on sensitization nucleocapsid
Application.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107376955A (en) * | 2017-07-28 | 2017-11-24 | 浙江师范大学 | A kind of photocatalysis antibacterial material and preparation method thereof |
| CN107640782A (en) * | 2017-09-26 | 2018-01-30 | 安徽省立医院 | A kind of brilliant preparation method of sub-10 nano calcirm-fluoride core-shell nano and its application in nuclear magnetic resonance |
| CN108557861A (en) * | 2018-05-28 | 2018-09-21 | 合肥国轩高科动力能源有限公司 | NaYF is converted in one kind4The preparation method of nano-powder self-assembled film |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103865538A (en) * | 2014-02-23 | 2014-06-18 | 复旦大学 | Up/down conversion dual-mode fluorescent nanomaterial for Nd<3+> sensitization and synthesis method thereof |
| WO2014116631A1 (en) * | 2013-01-22 | 2014-07-31 | University Of Massachusetts Medical School | Compositions and methods for upconverting luminescence with engineered excitation and applications thereof |
| CN105505374A (en) * | 2016-02-01 | 2016-04-20 | 东南大学 | Up-conversion luminescence composite material based on dye sensitization and preparation method of up-conversion luminescence composite material |
| CN106124458A (en) * | 2015-12-09 | 2016-11-16 | 南京工业大学 | A kind of method utilizing conversion nano granule to measure Water in Organic Solvents content |
-
2017
- 2017-03-08 CN CN201710133447.XA patent/CN106867509B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014116631A1 (en) * | 2013-01-22 | 2014-07-31 | University Of Massachusetts Medical School | Compositions and methods for upconverting luminescence with engineered excitation and applications thereof |
| CN103865538A (en) * | 2014-02-23 | 2014-06-18 | 复旦大学 | Up/down conversion dual-mode fluorescent nanomaterial for Nd<3+> sensitization and synthesis method thereof |
| CN106124458A (en) * | 2015-12-09 | 2016-11-16 | 南京工业大学 | A kind of method utilizing conversion nano granule to measure Water in Organic Solvents content |
| CN105505374A (en) * | 2016-02-01 | 2016-04-20 | 东南大学 | Up-conversion luminescence composite material based on dye sensitization and preparation method of up-conversion luminescence composite material |
Non-Patent Citations (2)
| Title |
|---|
| DAQIN CHEN ET AL: "Highly intense upconversion luminescence in Yb/Er:NaGdF4@NaYF4 core–shell nanocrystals with complete shell enclosure of the core", 《DALTON TRANS.》 * |
| L. MARCINIAK ET AL,: "A broadening temperature sensitivity range with a core– shell YbEr@YbNd double ratiometric optical nanothermometer", 《NANOSCALE》 * |
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| CN111320199A (en) * | 2020-03-24 | 2020-06-23 | 福建师范大学 | Anti-counterfeiting fluoride nanoparticle composite material and preparation method thereof |
| CN111320199B (en) * | 2020-03-24 | 2022-08-19 | 福建师范大学 | Anti-counterfeiting fluoride nanoparticle composite material and preparation method thereof |
| CN112358879A (en) * | 2020-12-04 | 2021-02-12 | 武汉工程大学 | Core-shell nano composite luminescent material and preparation method thereof |
| CN112358879B (en) * | 2020-12-04 | 2022-07-19 | 武汉工程大学 | Core-shell nano composite luminescent material and preparation method thereof |
| CN113549446A (en) * | 2021-07-09 | 2021-10-26 | 上海大学 | Neodymium-sensitized rare earth luminescent multilayer core-shell structure material, and preparation method and application thereof |
| CN113388402A (en) * | 2021-07-19 | 2021-09-14 | 南京邮电大学 | Double-excitation multicolor luminous rare earth up-conversion nanoparticles and preparation method thereof |
| CN116891742A (en) * | 2023-06-07 | 2023-10-17 | 西安邮电大学 | Rare earth luminescent material and preparation method and application thereof |
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