CN106010537B - The preparation of difunctional nano core-shell material is sensed with white light emission and light temperature - Google Patents
The preparation of difunctional nano core-shell material is sensed with white light emission and light temperature Download PDFInfo
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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
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
- C09K11/7772—Halogenides
- C09K11/7773—Halogenides with alkali or alkaline earth metal
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Abstract
The present invention relates to a kind of preparation that difunctional nano core-shell material is sensed with white light emission and light temperature, its chemical composition formula is NaYbF4:Nd3+@NaY1‑yF4:Yby 3+；The fluorescent material preparation method is as follows：Than accurately raw material is weighed by the chemical composition mol ratio of formula, it is put into three-neck flask and adds appropriate oleic acid and oleyl amine to be sufficiently stirred, logical argon gas, 120 DEG C of heating stirrings and constant temperature holding 30min, then 275 DEG C of holding 30min are being heated to, are being produced with alcohol washes after cooling and with centrifuge；The feux rouges and blue emission of nano core-shell material of the present invention are stronger, and high color purity, colour temperature is relatively low, is adapted to be prepared on a large scale, available for fields such as white light emission, light temperature sensing and biological fluorescent labelings.
Description
Technical field
The invention belongs to rare earth luminescent material technical field, and in particular to a kind of to be received with what white light emission and light temperature sensed
Rice material and preparation method thereof.
Background technology
White light up-conversion luminescent material be now widely used for solid three-dimensional show, the field such as biological fluorescent labeling, market
Have a extensive future.Realize that white light emission mainly there are two methods at present：When changed under frequency, second, control three kinds of light of RGB
Intensity.But white light emission realizes that most materials is glass ceramics, glass ceramics preparation section is cumbersome, and performance comparision
It is low, can not meet the needs of high performance device.Therefore strengthen the white light emission intensity of nano material, prepare new white-light nanometer
Material is to be highly desirable.
The content of the invention
The present invention, which provides one kind, has white light emission and light temperature sensing dual-functional nanometer core-shell material preparation method, chooses
NaYbF4The middle Nd for introducing appropriate concentration3+Ion is nanometer nuclear material, and carries out NaYF to it4:Yb3+Cladding utilizes thermal decomposition method
Form stable solid solution agent.Nd3+、Yb3+Introducing enhance energy conversion, improve Nd3+The absorption of ion pair infrared light, so as to
Improve blue and green light and red light-emitting intensity.
There is the present invention white light emission to sense difunctional nano core-shell material with light temperature, and its chemical general formula represents：
NaYbF4:Nd3+@NaY1-yF4:Yby 3+
Wherein：1%≤y≤100%.
There is the present invention white light emission and the preparation of light temperature sensing dual-functional nanometer core shell structure to be synthesized using Pintsch process
Method, specific preparation method are as follows：
A, by NaYbF4:Nd3+@NaY1-yF4:Yby 3+Chemical composition measure than accurately weighing following raw material：Trifluoroacetic acid
Sodium NaCF3The COO and Y that purity is more than 99.99%2O3、Yb2O3And Nd2O3；
B, the raw material in step a is added in three-neck flask, adds appropriate oleic acid and oleyl amine is sufficiently stirred, lead to argon gas,
And heat.Heating is divided into two stages：
First stage：After being heated to 120 DEG C, 120 DEG C of constant temperature keep 30min；
Second stage：After being heated to 275 DEG C, 275 DEG C of constant temperature keep 30min；
C, above-mentioned solution addition absolute ethyl alcohol centrifuge washing is produced into required product.
Beneficial effect：
(1) preparation method of the present invention is easy, and colour temperature is relatively low, is adapted to industrial mass manufacture.
(2) nano core-shell quality of materials produced by the present invention is higher, and colour temperature is relatively low.
(3) it is cheap, new.
(4) NaYbF of the present invention4And NaYF4Material is the new light-converting material that a kind of stability is good, colourity is good,
NaYF4:Yb3+Cladding enhance feux rouges and blue emission intensity, while enhance NaYbF4:Nd3+White light emission, swash ultraviolet
Give, luminous intensity is larger, and luminous efficient, high color purity.
Brief description of the drawings
Fig. 1 NaYbF4:2%Nd3+@NaYF4:1%Yb3+Emission spectrum in the case where 980nm light excites
Fig. 2 NaYbF4:2%Nd3+@NaYF4:3%Yb3+Emission spectrum in the case where 980nm light excites
Fig. 3 NaYbF4:2%Nd3+@NaYF4:4%Yb3+Emission spectrum in the case where 980nm light excites
Fig. 4 NaYbF4:2%Nd3+@NaYF4:5%Yb3+Emission spectrum in the case where 980nm light excites
Fig. 5 NaYbF4:2%Nd3+@NaYF4:6%Yb3+Emission spectrum in the case where 980nm light excites
Fig. 6 NaYbF4:2%Nd3+@NaYF4:8%Yb3+Emission spectrum in the case where 980nm light excites
Fig. 7 NaYbF4:2%Nd3+@NaYF4:10%Yb3+Emission spectrum in the case where 980nm light excites
Fig. 8 NaYbF4:2%Nd3+@NaYF4:20%Yb3+Emission spectrum in the case where 980nm light excites
Fig. 9 NaYbF4:2%Nd3+@NaYF4:30%Yb3+Emission spectrum in the case where 980nm light excites
Figure 10 NaYbF4:2%Nd3+@NaYF4:50%Yb3+Emission spectrum in the case where 980nm light excites
Figure 11 NaYbF4:2%Nd3+@Na Yb4Emission spectrum of the F in the case where 980nm light excites
Embodiment：
Embodiment 1：
The molecular formula of synthetic is NaYbF4:2%Nd3+@NaYF4:1%Yb3+.Weigh NaC3FCOO 0.1360g, Nd
(CF3COO)30.0079g, Yb (CF3COO)30.5091g, it is placed in three-neck flask, adds 16ml oleic acid and 8ml oleyl amines,
Argon gas is passed through, is stirred 15 minutes, 120 DEG C is heated to and is kept for 30 minutes, 275 DEG C is then again heated to and is kept for 30 minutes, it is cold
But centrifugation is washed with absolute ethyl alcohol afterwards, is finally putting into 70 DEG C of bakings in drying box and produces for 24 hours.Weigh what is prepared
NaYbF4:2%Nd3+0.1030g is put into beaker, adds 5ml hexamethylene, ultrasound 30 minutes, weighs NaCF3COO0.1360g,
Y (the CF prepared3COO)30.4237g, Yb (CF3COO)30.0050g is placed in three-neck flask, add 16ml oleic acid and
8ml oleyl amines, and by the good NaYbF of ultrasound4:2%Nd3+, cyclohexane solution adds in three-neck flask, is passed through argon gas, stirs 15 points
Clock, it is heated to 120 DEG C and is kept for 30 minutes, is then again heated to 275 DEG C and is kept for 30 minutes, washed after cooling with absolute ethyl alcohol
Centrifugation, it is finally putting into 70 DEG C of bakings in drying box and produces for 24 hours.Emission spectrum of the sample in the case where 980nm light excites is referring to Fig. 1.
Embodiment 2：
The molecular formula of synthetic is NaYbF4:2%Nd3+@NaYF4:3%Yb3+.Weigh NaC3FCOO 0.1360g, Nd
(CF3COO)30.0079g, Yb (CF3COO)30.5091g, it is placed in three-neck flask, adds 16ml oleic acid and 8ml oleyl amines,
Argon gas is passed through, is stirred 15 minutes, 120 DEG C is heated to and is kept for 30 minutes, 275 DEG C is then again heated to and is kept for 30 minutes, it is cold
But centrifugation is washed with absolute ethyl alcohol afterwards, is finally putting into 70 DEG C of bakings in drying box and produces for 24 hours.Weigh what is prepared
NaYbF4:2%Nd3+0.1030g is put into beaker, adds 5ml hexamethylene, ultrasound 30 minutes, weighs NaCF3COO0.1360g,
Y (the CF prepared3COO)30.4152g, Yb (CF3COO)30.0150g is placed in three-neck flask, add 16ml oleic acid and
8ml oleyl amines, and by the good NaYbF of ultrasound4:2%Nd3+, cyclohexane solution adds in three-neck flask, is passed through argon gas, stirs 15 points
Clock, it is heated to 120 DEG C and is kept for 30 minutes, is then again heated to 275 DEG C and is kept for 30 minutes, washed after cooling with absolute ethyl alcohol
Centrifugation, it is finally putting into 70 DEG C of bakings in drying box and produces for 24 hours.Emission spectrum of the sample in the case where 980nm light excites is referring to Fig. 2.
Embodiment 3：
The molecular formula of synthetic is NaYbF4:2%Nd3+@NaYF4:4%Yb3+.Weigh NaC3FCOO 0.1360g, Nd
(CF3COO)30.0079g, Yb (CF3COO)30.5091g, it is placed in three-neck flask, adds 16ml oleic acid and 8ml oleyl amines,
Argon gas is passed through, is stirred 15 minutes, 120 DEG C is heated to and is kept for 30 minutes, 275 DEG C is then again heated to and is kept for 30 minutes, it is cold
But centrifugation is washed with absolute ethyl alcohol afterwards, is finally putting into 70 DEG C of bakings in drying box and produces for 24 hours.Weigh what is prepared
NaYbF4:2%Nd3+0.1030g is put into beaker, adds 5ml hexamethylene, ultrasound 30 minutes, weighs NaCF3COO0.1360g,
Y (the CF prepared3COO)30.4109g, Yb (CF3COO)30.0200g is placed in three-neck flask, add 16ml oleic acid and
8ml oleyl amines, and by the good NaYbF of ultrasound4:2%Nd3+, cyclohexane solution adds in three-neck flask, is passed through argon gas, stirs 15 points
Clock, it is heated to 120 DEG C and is kept for 30 minutes, is then again heated to 275 DEG C and is kept for 30 minutes, washed after cooling with absolute ethyl alcohol
Centrifugation, it is finally putting into 70 DEG C of bakings in drying box and produces for 24 hours.Emission spectrum of the sample in the case where 980nm light excites is referring to Fig. 3.
Embodiment 4：
The molecular formula of synthetic is NaYbF4:2%Nd3+@NaYF4:5%Yb3+.Weigh NaC3FCOO 0.1360g, Nd
(CF3COO)30.0079g, Yb (CF3COO)30.5091g, it is placed in three-neck flask, adds 16ml oleic acid and 8ml oleyl amines,
Argon gas is passed through, is stirred 15 minutes, 120 DEG C is heated to and is kept for 30 minutes, 275 DEG C is then again heated to and is kept for 30 minutes, it is cold
But centrifugation is washed with absolute ethyl alcohol afterwards, is finally putting into 70 DEG C of bakings in drying box and produces for 24 hours.Weigh what is prepared
NaYbF4:2%Nd3+0.1030g is put into beaker, adds 5ml hexamethylene, ultrasound 30 minutes, weighs NaCF3COO0.1360g,
Y (the CF prepared3COO)30.4066g, Yb (CF3COO)30.0256g is placed in three-neck flask, add 16ml oleic acid and
8ml oleyl amines, and by the good NaYbF of ultrasound4:2%Nd3+, cyclohexane solution adds in three-neck flask, is passed through argon gas, stirs 15 points
Clock, it is heated to 120 DEG C and is kept for 30 minutes, is then again heated to 275 DEG C and is kept for 30 minutes, washed after cooling with absolute ethyl alcohol
Centrifugation, it is finally putting into 70 DEG C of bakings in drying box and produces for 24 hours.Emission spectrum of the sample in the case where 980nm light excites is referring to Fig. 4.
Embodiment 5：
The molecular formula of synthetic is NaYbF4:2%Nd3+@NaYF4:6%Yb3+.Weigh NaC3FCOO 0.1360g, Nd
(CF3COO)30.0079g, Yb (CF3COO)30.5091g, it is placed in three-neck flask, adds 16ml oleic acid and 8ml oleyl amines,
Argon gas is passed through, is stirred 15 minutes, 120 DEG C is heated to and is kept for 30 minutes, 275 DEG C is then again heated to and is kept for 30 minutes, it is cold
But centrifugation is washed with absolute ethyl alcohol afterwards, is finally putting into 70 DEG C of bakings in drying box and produces for 24 hours.Weigh what is prepared
NaYbF4:2%Nd3+0.1030g is put into beaker, adds 5ml hexamethylene, ultrasound 30 minutes, weighs NaCF3COO0.1360g,
Y (the CF prepared3COO)30.4023g, Yb (CF3COO)30.0300g is placed in three-neck flask, add 16ml oleic acid and
8ml oleyl amines, and by the good NaYbF of ultrasound4:2%Nd3+, cyclohexane solution adds in three-neck flask, is passed through argon gas, stirs 15 points
Clock, it is heated to 120 DEG C and is kept for 30 minutes, is then again heated to 275 DEG C and is kept for 30 minutes, washed after cooling with absolute ethyl alcohol
Centrifugation, it is finally putting into 70 DEG C of bakings in drying box and produces for 24 hours.Emission spectrum of the sample in the case where 980nm light excites is referring to Fig. 5.
Embodiment 6：
The molecular formula of synthetic is NaYbF4:2%Nd3+@NaYF4:8%Yb3+.Weigh NaC3FCOO 0.1360g, Nd
(CF3COO)30.0079g, Yb (CF3COO)30.5091g, it is placed in three-neck flask, adds 16ml oleic acid and 8ml oleyl amines,
Argon gas is passed through, is stirred 15 minutes, 120 DEG C is heated to and is kept for 30 minutes, 275 DEG C is then again heated to and is kept for 30 minutes, it is cold
But centrifugation is washed with absolute ethyl alcohol afterwards, is finally putting into 70 DEG C of bakings in drying box and produces for 24 hours.Weigh what is prepared
NaYbF4:2%Nd3+0.1030g is put into beaker, adds 5ml hexamethylene, ultrasound 30 minutes, weighs NaCF3COO0.1360g,
Y (the CF prepared3COO)30.3938g, Yb (CF3COO)30.0400g is placed in three-neck flask, add 16ml oleic acid and
8ml oleyl amines, and by the good NaYbF of ultrasound4:2%Nd3+, cyclohexane solution adds in three-neck flask, is passed through argon gas, stirs 15 points
Clock, it is heated to 120 DEG C and is kept for 30 minutes, is then again heated to 275 DEG C and is kept for 30 minutes, washed after cooling with absolute ethyl alcohol
Centrifugation, it is finally putting into 70 DEG C of bakings in drying box and produces for 24 hours.Emission spectrum of the sample in the case where 980nm light excites is referring to Fig. 6.
Embodiment 7：
The molecular formula of synthetic is NaYbF4:2%Nd3+@NaYF4:10%Yb3+.Weigh NaCF3COO 0.1360g, Nd
(CF3COO)30.0079g, Yb (CF3COO)30.5091g, it is placed in three-neck flask, adds 16ml oleic acid and 8ml oleyl amines,
Argon gas is passed through, is stirred 15 minutes, 120 DEG C is heated to and is kept for 30 minutes, 275 DEG C is then again heated to and is kept for 30 minutes, it is cold
But centrifugation is washed with absolute ethyl alcohol afterwards, is finally putting into 70 DEG C of bakings in drying box and produces for 24 hours.Weigh what is prepared
NaYbF4:2%Nd3+0.1030g is put into beaker, adds 5ml hexamethylene, ultrasound 30 minutes, weighs NaCF3COO0.1360g,
Y (the CF prepared3COO)30.3852g, Yb (CF3COO)30.0512g is placed in three-neck flask, add 16ml oleic acid and
8ml oleyl amines, and by the good NaYbF of ultrasound4:2%Nd3+, cyclohexane solution adds in three-neck flask, is passed through argon gas, stirs 15 points
Clock, it is heated to 120 DEG C and is kept for 30 minutes, is then again heated to 275 DEG C and is kept for 30 minutes, washed after cooling with absolute ethyl alcohol
Centrifugation, it is finally putting into 70 DEG C of bakings in drying box and produces for 24 hours.Emission spectrum of the sample in the case where 980nm light excites is referring to Fig. 7.
Embodiment 8：
The molecular formula of synthetic is NaYbF4:2%Nd3+@NaYF4:20%Yb3+.Weigh NaCF3COO 0.1360g, weigh
NaCF3COO 0.1360g, Nd (CF3COO)30.0079g, Yb (CF3COO)30.5091g, it is placed in three-neck flask, adds
16ml oleic acid and 8ml oleyl amines, argon gas is passed through, stirred 15 minutes, be heated to 120 DEG C and kept for 30 minutes, be then again heated to 275
DEG C and kept for 30 minutes, wash centrifugation with absolute ethyl alcohol after cooling, is finally putting into drying box 70 DEG C of bakings and produces for 24 hours.Weigh
The NaYbF prepared4:2%Nd3+0.1030g is put into beaker, adds 5ml hexamethylene, ultrasound 30 minutes, weighs
NaCF3COO 0.1360g, the Y (CF prepared3COO)30.3424g, Yb (CF3COO)30.1024g is placed on three-neck flask
In, add 16ml oleic acid and 8ml oleyl amines, and by the good NaYbF of ultrasound4:2%Nd3+, cyclohexane solution add three-neck flask in,
Argon gas is passed through, is stirred 15 minutes, 120 DEG C is heated to and is kept for 30 minutes, 275 DEG C is then again heated to and is kept for 30 minutes, it is cold
But centrifugation is washed with absolute ethyl alcohol afterwards, is finally putting into 70 DEG C of bakings in drying box and produces for 24 hours.Sample is in the case where 980nm light excites
Emission spectrum is referring to Fig. 8.
Embodiment 9：
The molecular formula of synthetic is NaYbF4:2%Nd3+@NaYF4:30%Yb3+.Weigh NaC3FCOO 0.1360g, Nd
(CF3COO)30.0079g, Yb (CF3COO)30.5091g, it is placed in three-neck flask, adds 16ml oleic acid and 8ml oleyl amines,
Argon gas is passed through, is stirred 15 minutes, 120 DEG C is heated to and is kept for 30 minutes, 275 DEG C is then again heated to and is kept for 30 minutes, it is cold
But centrifugation is washed with absolute ethyl alcohol afterwards, is finally putting into 70 DEG C of bakings in drying box and produces for 24 hours.Weigh what is prepared
NaYbF4:2%Nd3+0.1030g is put into beaker, adds 5ml hexamethylene, ultrasound 30 minutes, weighs NaCF3COO0.1360g,
Y (the CF prepared3COO)30.2996g, Yb (CF3COO)30.1536g is placed in three-neck flask, add 16ml oleic acid and
8ml oleyl amines, and by the good NaYbF of ultrasound4:2%Nd3+, cyclohexane solution adds in three-neck flask, is passed through argon gas, stirs 15 points
Clock, it is heated to 120 DEG C and is kept for 30 minutes, is then again heated to 275 DEG C and is kept for 30 minutes, washed after cooling with absolute ethyl alcohol
Centrifugation, it is finally putting into 70 DEG C of bakings in drying box and produces for 24 hours.Emission spectrum of the sample in the case where 980nm light excites is referring to Fig. 9.
Embodiment 10：
The molecular formula of synthetic is NaYbF4:2%Nd3+@NaYF4:50%Yb3+.Weigh NaC3FCOO 0.1360g, Nd
(CF3COO)30.0079g, Yb (CF3COO)30.5091g, it is placed in three-neck flask, adds 16ml oleic acid and 8ml oleyl amines,
Argon gas is passed through, is stirred 15 minutes, 120 DEG C is heated to and is kept for 30 minutes, 275 DEG C is then again heated to and is kept for 30 minutes, it is cold
But centrifugation is washed with absolute ethyl alcohol afterwards, is finally putting into 70 DEG C of bakings in drying box and produces for 24 hours.Weigh what is prepared
NaYbF4:2%Nd3+0.1030g is put into beaker, adds 5ml hexamethylene, ultrasound 30 minutes, weighs NaCF3COO0.1360g, Y
(CF3COO)30.2140g, Yb (CF3COO)30.2500g, it is placed in three-neck flask, adds 16ml oleic acid and 8ml oleyl amines,
And by the good NaYbF of ultrasound4:2%Nd3+, cyclohexane solution adds in three-neck flask, is passed through argon gas, stirs 15 minutes, be heated to
120 DEG C are kept for 30 minutes, are then again heated to 275 DEG C and are kept for 30 minutes, wash centrifugation with absolute ethyl alcohol after cooling, finally
70 DEG C of bakings in drying box are put into produce within 24 hours.Emission spectrum of the sample in the case where 980nm light excites is referring to Figure 10.
Embodiment 11：
The molecular formula of synthetic is NaYbF4:2%Nd3+@NaYbF4.Weigh NaCF3COO 0.1360g, Nd (CF3COO)30.0079g, Yb (CF3COO)30.5091g, it is placed in three-neck flask, adds 16ml oleic acid and 8ml oleyl amines, be passed through argon gas,
Stirring 15 minutes, it is heated to 120 DEG C and is kept for 30 minutes, is then again heated to 275 DEG C and is kept for 30 minutes, with anhydrous after cooling
Ethanol washing centrifugation, it is finally putting into 70 DEG C of bakings in drying box and produces for 24 hours.Weigh the NaYbF prepared4:2%Nd3+
0.1030g is put into beaker, adds 5ml hexamethylene, ultrasound 30 minutes, weighs NaCF3COO0.1360g, Yb (CF3COO)3
0.5121g, it is placed in three-neck flask, adds 16ml oleic acid and 8ml oleyl amines, and by the good NaYbF of ultrasound4:2%Nd3+, ring
Hexane solution is added in three-neck flask, is passed through argon gas, is stirred 15 minutes, is heated to 120 DEG C and is kept for 30 minutes, is then heated again
To 275 DEG C and kept for 30 minutes, centrifugation wash with absolute ethyl alcohol after cooling, be finally putting into drying box 70 DEG C of bakings 24 hours i.e.
.Emission spectrum of the sample in the case where 980nm light excites is referring to Figure 11.
Claims (1)
1. one kind has white light emission and light temperature sensing dual-functional nanometer core-shell material, it is characterised in that chemical composition is led to following
Formula represents：
NaYbF4:Nd3+@NaY1-yF4:Yby 3+
Wherein：1%≤y≤100%.
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