CN106010537A - Preparation method of core-shell nanomaterial with white light emitting and light and temperature sensing double functions - Google Patents

Preparation method of core-shell nanomaterial with white light emitting and light and temperature sensing double functions Download PDF

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CN106010537A
CN106010537A CN201610369038.5A CN201610369038A CN106010537A CN 106010537 A CN106010537 A CN 106010537A CN 201610369038 A CN201610369038 A CN 201610369038A CN 106010537 A CN106010537 A CN 106010537A
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CN106010537B (en
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王祥夫
徐同同
步妍妍
颜晓红
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Nanjing Post and Telecommunication University
Nanjing University of Posts and Telecommunications
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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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
    • Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps

Abstract

The invention relates to a preparation method of a core-shell nanomaterial with white light emitting and light and temperature sensing double functions. The general formula of the chemical composition of the nanomaterial is NaYbF4:Nd<3+>@NaY1-yF4:Yby<3+>. The preparation method of the above phosphor comprises the following steps: accurately weighing raw materials according to the chemical composition mole ratio of the general formula, putting the weighed raw materials in a three-necked flask, adding a proper amount of oleic acid and oleylamine, fully stirring all above materials, introducing argon, heating and stirring above materials to 120DEG C, keeping the temperature unchanged for 30min, heating the materials to 275DEG C, keeping the temperature unchanged for 30min, cooling the above obtained material, cleaning the cooled material with alcohol, and centrifuging the cleaned material through a centrifuge to obtain the core-shell nanomaterial. The core-shell nanomaterial has the advantages of strong red and blue light emission, good color purity, low color temperature, and suitableness for large-batch preparation, and can be used in the fields of white light emission, light and temperature sensing and fluorescence probes.

Description

There is white light emission and the preparation of the light temperature bifunctional nano core-shell material of sensing
Technical field
The invention belongs to rare earth luminescent material technical field, be specifically related to a kind of have white light emission and light temperature sensing receive 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 white light emission at present and mainly have two kinds of methods: one is to change under frequency, and two is to control three kinds of light of RGB Intensity.But it is glass ceramics that white light emission realizes most materials, glass ceramics preparation section is loaded down with trivial details, and Performance comparision Low, it is impossible to meet the demand of high performance device.Therefore strengthen the white light emission intensity of nano material, prepare novel white-light nanometer Material is to be highly desirable to.
Summary of the invention
The present invention provides one to have white light emission and senses dual-functional nanometer core-shell material preparation method with light temperature, chooses NaYbF4The Nd of the appropriate concentration of middle introducing3+Ion is nanometer nuclear material, and it is carried out NaYF4: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, thus Improve blue and green light and red light-emitting intensity.
The present invention has white light emission and senses bifunctional nano core-shell material with light temperature, and its chemical general formula represents:
NaYbF4:Nd3+@NaY1-yF4:Yby 3+
Wherein: 1≤y≤100%.
The present invention has the preparation employing Pintsch process synthesis of white light emission and light temperature sensing dual-functional nanometer nucleocapsid structure Method, concrete preparation method is as follows:
A, by NaYbF4:Nd3+@NaY1-yF4:Yby 3+Chemical composition metering than accurately weighing following raw material: sodium acetate NaCF3COO and purity are the Y of more than 99.99%2O3、Yb2O3And Nd2O3；
B, the raw material in step a is added in three-neck flask, add appropriate oleic acid and oleyl amine is sufficiently stirred for, logical argon, And heat.Heat and be 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, by above-mentioned solution addition dehydrated alcohol centrifuge washing i.e. obtain required product.
Beneficial effect:
(1) preparation method of the present invention is easy, and colour temperature is relatively low, is suitable for industrial mass manufacture.
(2) the nano core-shell quality of materials that the present invention prepares is higher, and colour temperature is on the low side.
(3) cheap, novel.
(4) NaYbF that the present invention relates to4And NaYF4Material is the novel light-converting material that a kind of good stability, colourity are good, NaYF4:Yb3+Cladding enhance HONGGUANG and blue emission intensity, enhance NaYbF simultaneously4:Nd3+White light emission, swashs in ultraviolet Giving, luminous intensity is relatively big, and luminous efficient, high color purity.
Accompanying drawing explanation
Fig. 1 NaYbF4: 2%Nd3+@NaYF4: 1%Yb3+Emission spectrum under 980nm light excites
Fig. 2 NaYbF4: 2%Nd3+@NaYF4: 3%Yb3+Emission spectrum under 980nm light excites
Fig. 3 NaYbF4: 2%Nd3+@NaYF4: 4%Yb3+Emission spectrum under 980nm light excites
Fig. 4 NaYbF4: 2%Nd3+@NaYF4: 5%Yb3+Emission spectrum under 980nm light excites
Fig. 5 NaYbF4: 2%Nd3+@NaYF4: 6%Yb3+Emission spectrum under 980nm light excites
Fig. 6 NaYbF4: 2%Nd3+@NaYF4: 8%Yb3+Emission spectrum under 980nm light excites
Fig. 7 NaYbF4: 2%Nd3+@NaYF4: 10%Yb3+Emission spectrum under 980nm light excites
Fig. 8 NaYbF4: 2%Nd3+@NaYF4: 20%Yb3+Emission spectrum under 980nm light excites
Fig. 9 NaYbF4: 2%Nd3+@NaYF4: 30%Yb3+Emission spectrum under 980nm light excites
Figure 10 NaYbF4: 2%Nd3+@NaYF4: 50%Yb3+Emission spectrum under 980nm light excites
Figure 11 NaYbF4: 2%Nd3+@NaYbF4Emission spectrum under 980nm light excites
Detailed description of the invention:
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, is placed in three-neck flask, adds 16ml oleic acid and 8ml oleyl amine, It is passed through argon, stirs 15 minutes, be heated to 120 DEG C and keep 30 minutes, be again heated to 275 DEG C subsequently and keep 30 minutes, cold It is centrifuged with absolute ethanol washing the most afterwards, is finally putting in drying baker 70 DEG C and dries 24 hours and get final product.Weighing has prepared NaYbF4: 2%Nd3+0.1030g puts into beaker, adds the hexamethylene of 5ml, has children outside the state plan 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 amine, and by ultrasonic good NaYbF4: 2%Nd3+, cyclohexane solution adds in three-neck flask, is passed through argon, stirs 15 points Clock, is heated to 120 DEG C and keeps 30 minutes, be again heated to 275 DEG C subsequently and keep 30 minutes, using absolute ethanol washing after cooling Centrifugal, it is finally putting in drying baker 70 DEG C and dries 24 hours and get final product.Sample emission spectrum under 980nm light excites sees 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, is placed in three-neck flask, adds 16ml oleic acid and 8ml oleyl amine, It is passed through argon, stirs 15 minutes, be heated to 120 DEG C and keep 30 minutes, be again heated to 275 DEG C subsequently and keep 30 minutes, cold It is centrifuged with absolute ethanol washing the most afterwards, is finally putting in drying baker 70 DEG C and dries 24 hours and get final product.Weighing has prepared NaYbF4: 2%Nd3+0.1030g puts into beaker, adds the hexamethylene of 5ml, has children outside the state plan 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 amine, and by ultrasonic good NaYbF4: 2%Nd3+, cyclohexane solution adds in three-neck flask, is passed through argon, stirs 15 points Clock, is heated to 120 DEG C and keeps 30 minutes, be again heated to 275 DEG C subsequently and keep 30 minutes, using absolute ethanol washing after cooling Centrifugal, it is finally putting in drying baker 70 DEG C and dries 24 hours and get final product.Sample emission spectrum under 980nm light excites sees 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, is placed in three-neck flask, adds 16ml oleic acid and 8ml oleyl amine, It is passed through argon, stirs 15 minutes, be heated to 120 DEG C and keep 30 minutes, be again heated to 275 DEG C subsequently and keep 30 minutes, cold It is centrifuged with absolute ethanol washing the most afterwards, is finally putting in drying baker 70 DEG C and dries 24 hours and get final product.Weighing has prepared NaYbF4: 2%Nd3+0.1030g puts into beaker, adds the hexamethylene of 5ml, has children outside the state plan 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 amine, and by ultrasonic good NaYbF4: 2%Nd3+, cyclohexane solution adds in three-neck flask, is passed through argon, stirs 15 points Clock, is heated to 120 DEG C and keeps 30 minutes, be again heated to 275 DEG C subsequently and keep 30 minutes, using absolute ethanol washing after cooling Centrifugal, it is finally putting in drying baker 70 DEG C and dries 24 hours and get final product.Sample emission spectrum under 980nm light excites sees 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, is placed in three-neck flask, adds 16ml oleic acid and 8ml oleyl amine, It is passed through argon, stirs 15 minutes, be heated to 120 DEG C and keep 30 minutes, be again heated to 275 DEG C subsequently and keep 30 minutes, cold It is centrifuged with absolute ethanol washing the most afterwards, is finally putting in drying baker 70 DEG C and dries 24 hours and get final product.Weighing has prepared NaYbF4: 2%Nd3+0.1030g puts into beaker, adds the hexamethylene of 5ml, has children outside the state plan 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 amine, and by ultrasonic good NaYbF4: 2%Nd3+, cyclohexane solution adds in three-neck flask, is passed through argon, stirs 15 points Clock, is heated to 120 DEG C and keeps 30 minutes, be again heated to 275 DEG C subsequently and keep 30 minutes, using absolute ethanol washing after cooling Centrifugal, it is finally putting in drying baker 70 DEG C and dries 24 hours and get final product.Sample emission spectrum under 980nm light excites sees 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, is placed in three-neck flask, adds 16ml oleic acid and 8ml oleyl amine, It is passed through argon, stirs 15 minutes, be heated to 120 DEG C and keep 30 minutes, be again heated to 275 DEG C subsequently and keep 30 minutes, cold It is centrifuged with absolute ethanol washing the most afterwards, is finally putting in drying baker 70 DEG C and dries 24 hours and get final product.Weighing has prepared NaYbF4: 2%Nd3+0.1030g puts into beaker, adds the hexamethylene of 5ml, has children outside the state plan 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 amine, and by ultrasonic good NaYbF4: 2%Nd3+, cyclohexane solution adds in three-neck flask, is passed through argon, stirs 15 points Clock, is heated to 120 DEG C and keeps 30 minutes, be again heated to 275 DEG C subsequently and keep 30 minutes, using absolute ethanol washing after cooling Centrifugal, it is finally putting in drying baker 70 DEG C and dries 24 hours and get final product.Sample excitation spectrum under 980nm light excites sees 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, is placed in three-neck flask, adds 16ml oleic acid and 8ml oleyl amine, It is passed through argon, stirs 15 minutes, be heated to 120 DEG C and keep 30 minutes, be again heated to 275 DEG C subsequently and keep 30 minutes, cold It is centrifuged with absolute ethanol washing the most afterwards, is finally putting in drying baker 70 DEG C and dries 24 hours and get final product.Weighing has prepared NaYbF4: 2%Nd3+0.1030g puts into beaker, adds the hexamethylene of 5ml, has children outside the state plan 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 amine, and by ultrasonic good NaYbF4: 2%Nd3+, cyclohexane solution adds in three-neck flask, is passed through argon, stirs 15 points Clock, is heated to 120 DEG C and keeps 30 minutes, be again heated to 275 DEG C subsequently and keep 30 minutes, using absolute ethanol washing after cooling Centrifugal, it is finally putting in drying baker 70 DEG C and dries 24 hours and get final product.Sample excitation spectrum under 980nm light excites sees Fig. 6.
Embodiment 7:
The molecular formula of synthetic is NaYbF4: 2%Nd3+@NaYF4: 10%Yb3+.Weigh NaC3FCOO 0.1360g, Nd (CF3COO)30.0079g, Yb (CF3COO)30.5091g, is placed in three-neck flask, adds 16ml oleic acid and 8ml oleyl amine, It is passed through argon, stirs 15 minutes, be heated to 120 DEG C and keep 30 minutes, be again heated to 275 DEG C subsequently and keep 30 minutes, cold It is centrifuged with absolute ethanol washing the most afterwards, is finally putting in drying baker 70 DEG C and dries 24 hours and get final product.Weighing has prepared NaYbF4: 2%Nd3+0.1030g puts into beaker, adds the hexamethylene of 5ml, has children outside the state plan 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 amine, and by ultrasonic good NaYbF4: 2%Nd3+, cyclohexane solution adds in three-neck flask, is passed through argon, stirs 15 points Clock, is heated to 120 DEG C and keeps 30 minutes, be again heated to 275 DEG C subsequently and keep 30 minutes, using absolute ethanol washing after cooling Centrifugal, it is finally putting in drying baker 70 DEG C and dries 24 hours and get final product.Sample excitation spectrum under 980nm light excites sees Fig. 7.
Embodiment 8:
The molecular formula of synthetic is NaYbF4: 2%Nd3+@NaYF4: 20%Yb3+.Weigh NaCF3COO 0.1360g, weighs NaCF3COO 0.1360g, Nd (CF3COO)30.0079g, Yb (CF3COO)30.5091g, is placed in three-neck flask, adds 16ml oleic acid and 8ml oleyl amine, be passed through argon, stirs 15 minutes, is heated to 120 DEG C and keeps 30 minutes, is again heated to 275 subsequently DEG C and keep 30 minutes, be centrifuged with absolute ethanol washing after cooling, be finally putting in drying baker 70 DEG C and dry 24 hours and get final product.Weigh The NaYbF prepared4: 2%Nd3+0.1030g puts into beaker, adds the hexamethylene of 5ml, has children outside the state plan 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 amine, and by ultrasonic good NaYbF4: 2%Nd3+, cyclohexane solution adds in three-neck flask, It is passed through argon, stirs 15 minutes, be heated to 120 DEG C and keep 30 minutes, be again heated to 275 DEG C subsequently and keep 30 minutes, cold It is centrifuged with absolute ethanol washing the most afterwards, is finally putting in drying baker 70 DEG C and dries 24 hours and get final product.Sample is under 980nm light excites Excitation spectrum sees 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, is placed in three-neck flask, adds 16ml oleic acid and 8ml oleyl amine, It is passed through argon, stirs 15 minutes, be heated to 120 DEG C and keep 30 minutes, be again heated to 275 DEG C subsequently and keep 30 minutes, cold It is centrifuged with absolute ethanol washing the most afterwards, is finally putting in drying baker 70 DEG C and dries 24 hours and get final product.Weighing has prepared NaYbF4: 2%Nd3+0.1030g puts into beaker, adds the hexamethylene of 5ml, has children outside the state plan 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 amine, and by ultrasonic good NaYbF4: 2%Nd3+, cyclohexane solution adds in three-neck flask, is passed through argon, stirs 15 points Clock, is heated to 120 DEG C and keeps 30 minutes, be again heated to 275 DEG C subsequently and keep 30 minutes, using absolute ethanol washing after cooling Centrifugal, it is finally putting in drying baker 70 DEG C and dries 24 hours and get final product.Sample excitation spectrum under 980nm light excites sees 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, is placed in three-neck flask, adds 16ml oleic acid and 8ml oleyl amine, It is passed through argon, stirs 15 minutes, be heated to 120 DEG C and keep 30 minutes, be again heated to 275 DEG C subsequently and keep 30 minutes, cold It is centrifuged with absolute ethanol washing the most afterwards, is finally putting in drying baker 70 DEG C and dries 24 hours and get final product.Weighing has prepared NaYbF4: 2%Nd3+0.1030g puts into beaker, adds the hexamethylene of 5ml, has children outside the state plan 30 minutes, weighs NaCF3COO0.1360g, Y (CF3COO)30.2140g, Yb (CF3COO)30.2500g, is placed in three-neck flask, adds 16ml oleic acid and 8ml oleyl amine, And by ultrasonic good NaYbF4: 2%Nd3+, cyclohexane solution adds in three-neck flask, is passed through argon, stirs 15 minutes, be heated to 120 DEG C keep 30 minutes, are again heated to 275 DEG C subsequently and keep 30 minutes, are centrifuged, finally with absolute ethanol washing after cooling Put in drying baker 70 DEG C dry 24 hours and get final product.Sample excitation spectrum under 980nm light excites sees 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, is placed in three-neck flask, adds 16ml oleic acid and 8ml oleyl amine, is passed through argon, Stir 15 minutes, be heated to 120 DEG C and keep 30 minutes, be again heated to 275 DEG C subsequently and keep 30 minutes, with anhydrous after cooling Washing with alcohol is centrifuged, and is finally putting in drying baker 70 DEG C and dries 24 hours and get final product.Weigh the NaYbF prepared4: 2%Nd3+ 0.1030g puts into beaker, adds the hexamethylene of 5ml, has children outside the state plan 30 minutes, weighs NaCF3COO0.1360g, Yb (CF3COO)3 0.5121g, is placed in three-neck flask, adds 16ml oleic acid and 8ml oleyl amine, and by ultrasonic good NaYbF4: 2%Nd3+, ring Hexane solution adds in three-neck flask, is passed through argon, stirs 15 minutes, is heated to 120 DEG C and keeps 30 minutes, the most again heats To 275 DEG C and keep 30 minutes, it is centrifuged with absolute ethanol washing after cooling, is finally putting in drying baker 70 DEG C and dries 24 hours i.e. ?.Sample excitation spectrum under 980nm light excites sees Figure 11.

Claims (4)

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 with following logical Formula represents:
NaYbF4:Nd3+@NaY1-yF4:Yby 3+
Wherein: 1≤y≤100%.
2. there is the preparation method of white light emission and light temperature sensing dual-functional nanometer core-shell material, it is characterised in that include following step Rapid:
A, respectively with acetate, rare earth oxide as raw material, according to chemical general formula NaYbF4:Nd3+@NaY1-yF4:Yby 3+Count respectively Calculate, weigh acetate and rare-earth oxidation compound；
B, the raw material in step a is added in three-neck flask, add appropriate oleic acid and oleyl amine is sufficiently stirred for, be passed through argon, and Heating.Heat and be divided into two stages:
First stage: after being heated to 120 DEG C, constant temperature keeps；
Second stage: after being heated to 275 DEG C, constant temperature keeps；
C, by above-mentioned solution addition dehydrated alcohol centrifuge washing i.e. obtain required product.
The preparation method with white light emission and light temperature sensing dual-functional nanometer core-shell material the most according to claim 2, It is characterized in that acetate used is NaCF3COO, rare earth oxide used is Y2O3,Yb2O3, Nd2O3。
The preparation method with white light emission and light temperature sensing dual-functional nanometer core-shell material the most according to claim 2, It is characterized in that the mixing of the raw material in step b is placed in three-neck flask, add oleic acid and oleyl amine stirs 0.25 hour so that it is uniformly mix Close.
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