CN104592994B - A kind of preparation method of the dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder of triangle - Google Patents
A kind of preparation method of the dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder of triangle Download PDFInfo
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Abstract
A kind of preparation method of the dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder of triangle disclosed by the invention, comprises the following steps:A) lanthanum salt and rare-earth europium salt are dissolved in mixing liquid and the stirring of diglycol and water;B) mixing liquid described in one side whipping step a) is while add urea and polyvinylpyrrolidone, until urea is completely dissolved to obtain colourless transparent liquid;C) colourless transparent liquid described in step b) is transferred under autoclave and reacted, obtain the europium doping dendritic lanthanum hydroxycarbonate of triangle.The method of the invention has the advantages that:(1) cost of material is low, synthesis technique is simple, product quality is stable and process repeatability can be good;(2) can extensive industrialization;(3) the strong red emission of product.Product prepared by methods described can be widely applied to agricultural film light conversion agent, PDP, LED fluorescent material and other high-tech areas.
Description
Technical field
The present invention relates to red embedded photoluminescent material field, more particularly to a kind of dendritic europium doping lanthanum hydroxycarbonate of triangle is red
The preparation method of color fluorescent material.
Background technology
Agricultural is the basis of the national economy in China, and China's economy can be promoted by further improving Crop yield and quality
Develop in a healthy way.Compared with the external conditions such as the cultivation and fertilising of crops, wherein light conversion film technology promotes crops fully sharp
Strengthen photosynthesis with the sun, not only had economic benefit but also there is environment protection significance.High energy UV is especially converted into Plant Light
The conversion film of the blood orange light of cooperation gains great popularity.The rare earth inorganic fluorescent material light conversion agent energy of light altering film for agriculture will be ultraviolet at present
Light is converted into blood orange light, and production cost is relatively low, and has stronger luminescent properties and ageing-resistant function.
Influenceing the factor of light-emitting phosphor efficiency includes the crystal structure of matrix, the doping concentration of rare earth ion and its distribution
State, the particle diameter of luminescent material and its pattern etc..Therefore, a luminous strong centre of luminescence and the good hair of optical property are selected
Light matrix is particularly important.Europium ion has stronger red emission in 620nm or so, and commonly selected is as red fluorescence material
The centre of luminescence;In addition, because lanthanum hydroxycarbonate possesses good hexagonal phase crystal structure and physical property, also commonly selected is as red
The luminous host of color fluorescent material and the presoma for preparing lanthanum hydroxide and lanthana, and by forerunner La (CO)3OH
Heat treatment, can obtain thermodynamically more stable La (OH)3And La2O3.So far, rear-earth-doped La (CO)3OH fluorescent material leads to
Prepared frequently with the precipitation method, sol-gel methods, template-directing method, microemulsion method and hydro-thermal method etc., gained sample majority is hexagonal phase
Structure.Therefore, to obtain the more excellent red fluorescence material of optical property, that seeks a kind of simple preparation hexagonal phase mixes europium La
(CO)3OH method seems particularly critical.
In recent years, with the development of farming technology, various agricultural functional materials are increasingly to low cost and high-quality
Direction is developed, and puts forward higher requirement to function agricultural material.Doping vario-property, which turns into, improves rear-earth-doped La (CO)3OH materials
A kind of effective means of optical property.Mix europium La (CO)3The particle diameters of OH red fluorescence materials, pattern, chemical composition and particle
Dispersity etc. all has a strong impact on its optical property and physical property and the application in light altering film for agriculture.Therefore, how to close
It is also the break-through point of prior art into the dendritic europium doping lanthanum hydroxycarbonate fluorescent material of granule regularizing triangle.
The content of the invention
A kind of low in raw material price is provided it is an object of the invention to overcome the deficiencies in the prior art, target product can
Control, preparation technology are simple, have good red emission and are easy to industrial red fluorescence powder, preparation method thereof.
To achieve the above object, the technical scheme taken of the present invention is:A kind of dendritic europium doping lanthanum hydroxycarbonate of triangle is red
The preparation method of color fluorescent material, comprises the following steps:
A) lanthanum salt and rare-earth europium salt are dissolved in mixed solution and the stirring of diglycol and water, the lanthanum salt and rare earth
The mol ratio of europium metal salt is 1:X, wherein 0<x<0.1;The volume ratio of water and diglycol is 1:Y, wherein 0.1<y<2;
B) mixing liquid described in one side whipping step a) is while add urea and polyvinylpyrrolidone, until urea is complete
Fully dissolved obtains colourless transparent liquid;
C) colourless transparent liquid described in step b) is transferred under autoclave in reaction, obtains linen triangle
Dendritic europium adulterates lanthanum hydroxycarbonate red fluorescence powder.
Being preferable to carry out for the preparation method of lanthanum hydroxycarbonate red fluorescence powder is adulterated as the dendritic europium of triangle of the present invention
Mode, the europium metal salt are one kind in europium nitrate or corresponding chloride.
Being preferable to carry out for the preparation method of lanthanum hydroxycarbonate red fluorescence powder is adulterated as the dendritic europium of triangle of the present invention
Mode, the lanthanum salt are at least one of lanthanum nitrate, lanthanum chloride, lanthanum sulfate, lanthanum acetate.
Being preferable to carry out for the preparation method of lanthanum hydroxycarbonate red fluorescence powder is adulterated as the dendritic europium of triangle of the present invention
Mode, the volume ratio of the water and diglycol is 1:0.5~1:1.5.
Being preferable to carry out for the preparation method of lanthanum hydroxycarbonate red fluorescence powder is adulterated as the dendritic europium of triangle of the present invention
The mol ratio of mode, the lanthanum salt and polyvinylpyrrolidone is 1:0.1~1:1.
Being preferable to carry out for the preparation method of lanthanum hydroxycarbonate red fluorescence powder is adulterated as the dendritic europium of triangle of the present invention
The mol ratio of mode, the lanthanum salt and urea is 1:2~1:4.
Being preferable to carry out for the preparation method of lanthanum hydroxycarbonate red fluorescence powder is adulterated as the dendritic europium of triangle of the present invention
Mode, step c) the mesohigh reactors volume is 30ml, and hydrothermal temperature is in 140 DEG C~200 DEG C, reaction time
12h~72h.
In invention, polyvinylpyrrolidone dissolving is used as a kind of soft mode version in the solution, is grown in lanthanum hydroxycarbonate
Adsorbed in journey in its anisotropic growth of lanthanum hydroxycarbonate spatial induction, finally enable and mix europium lanthanum hydroxycarbonate self assembly shape
Into triangle dendritic morphology.
A kind of preparation method of the dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder of triangle of the present invention, has following beneficial to effect
Fruit:
(1) raw material of preparation method provided by the invention is cheap and easy to get, and cost is low, and synthesis technique is simply easily realized, product
Steady quality and process repeatability can be good;
(2) present invention can realize the large-scale preparation of rare-earth europium doping lanthanum hydroxycarbonate;
(3) product has strong red emission.To sum up advantage, product prepared by methods described can be widely applied to agriculture
With film light conversion agent, PDP, LED fluorescent material and other high-tech areas.
Brief description of the drawings
Fig. 1 is the X ray of the dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder of triangle prepared by embodiments of the invention 1
Diffraction pattern.
Fig. 2 is the scanning of the dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder of triangle prepared by embodiments of the invention 1
Electron microscope.
Fig. 3 is the room temperature of the dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder of triangle prepared by embodiments of the invention 1
Fluorescence emission spectrum.
Embodiment
To better illustrate the object, technical solutions and advantages of the present invention, below in conjunction with the drawings and specific embodiments pair
The present invention is described further.
Embodiment 1
The preparation of the dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder of triangle, comprises the following steps:
A) appropriate lanthanum nitrate and the europium nitrate stirring and dissolving in the mixed solution of water and diglycol are weighed respectively, are made
It is 1 that lanthanum nitrate, which is obtained, with europium nitrate mol ratio:0.05, the volume ratio of water and diglycol is 1:0.8, then it will be weighed
Lanthanum nitrate and europium nitrate are dissolved in the mixed solution of water and diglycol;
B) mixing liquid described in one side whipping step a) is while add urea and polyvinylpyrrolidone so that lanthanum nitrate
Mol ratio with polyvinylpyrrolidone is 1:0.3, the mol ratio for obtaining lanthanum nitrate and urea is 1:2;Then the urine that will be weighed
Element and polyvinylpyrrolidone are dissolved in mixed solution and stir to clarify liquid;
C) clarified solution described in step b) is transferred to after being reacted 24 hours at 180 DEG C in 30ml high-temperature high-pressure reaction kettles
Obtain the dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder of triangle.
The dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder of gained triangle is accredited as hexagonal phase hydroxyl through X-ray powder diffraction
Lanthanum carbonate, powder x-ray diffraction result are as shown in Figure 1;Material morphology is obtained by ESEM result, as shown in Figure 2.Such as figure
2 can be seen that material granule is regular, and particle is in triangle dendritic morphology;Fig. 3 is the Room temperature PL spectrum of the sample, and the dendritic europium of triangle is mixed
Miscellaneous lanthanum hydroxycarbonate 262nm wavelength lights excite it is lower have emission peak at 593nm, 619nm, 650nm and 793nm respectively, it is and red
Color luminous intensity is maximum at 619nm.
Embodiment 2
The preparation of the dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder of triangle, comprises the following steps:
A) weigh appropriate lanthanum nitrate and europium nitrate respectively to stir in the mixed solution of water and diglycol so that nitre
Sour lanthanum is 1 with europium nitrate mol ratio:0.08, the volume ratio of water and diglycol is 1:1, the lanthanum nitrate that then will be weighed
The mixed solution of water and diglycol is dissolved in europium nitrate;
B) mixing liquid described in one side whipping step a) is while add urea and polyvinylpyrrolidone so that lanthanum nitrate
With being 1 with the mol ratio of polyvinylpyrrolidone:0.5, lanthanum nitrate is obtained with being 1 with the mol ratio of urea:3;Then will be weighed
Urea and polyvinylpyrrolidone be dissolved in mixed solution and stir to clarify liquid;
C) clarified solution described in step b) is transferred to after being reacted 24 hours at 190 DEG C in 30ml high-temperature high-pressure reaction kettles
Obtain the europium doping dendritic lanthanum hydroxycarbonate red fluorescence powder of triangle.
Gained triangle dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder through X-ray powder diffraction, ESEM identification with
And Room temperature PL spectrum (the dendritic europium doping lanthanum hydroxycarbonate of triangle prepared with embodiment 1 is similar), it is known that it is that triangle is dendritic
Europium adulterates lanthanum hydroxycarbonate.
Embodiment 3
The preparation of the dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder of triangle, comprises the following steps:
A) weigh appropriate lanthanum nitrate and europium nitrate respectively to stir in the mixed solution of water and diglycol so that nitre
Sour lanthanum is 1 with europium nitrate mol ratio:0.09, the volume ratio of water and diglycol is 1:0.5, the nitric acid that then will be weighed
Lanthanum and europium nitrate are dissolved in the mixed solution of water and diglycol;
B) mixing liquid described in one side whipping step a) is while add urea and polyvinylpyrrolidone so that lanthanum nitrate
With being 1 with the mol ratio of polyvinylpyrrolidone:0.5, lanthanum nitrate is obtained with being 1 with the mol ratio of urea:2.5;Then by alleged by
The urea and polyvinylpyrrolidone taken is dissolved in mixed solution and stirs to clarify liquid;
C) clarified solution described in step b) is transferred to after being reacted 48 hours at 180 DEG C in 30ml high-temperature high-pressure reaction kettles
Obtain the dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder of triangle.
Gained triangle dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder through X-ray powder diffraction, ESEM identification with
And Room temperature PL spectrum (the dendritic europium doping lanthanum hydroxycarbonate of triangle prepared with embodiment 1 is similar), it is known that it is that triangle is dendritic
Europium adulterates lanthanum hydroxycarbonate.
Embodiment 4
Europium adulterates the preparation of the dendritic lanthanum hydroxycarbonate red fluorescence powder of triangle, comprises the following steps:
A) appropriate lanthanum nitrate and the europium nitrate stirring and dissolving in the mixed solution of water and diglycol are weighed respectively, are made
It is 1 that lanthanum nitrate, which is obtained, with europium nitrate mol ratio:0.05, the volume ratio of water and diglycol is 1:1.3 then it will be weighed
Lanthanum nitrate and europium nitrate are dissolved in the mixed solution of water and diglycol;
B) mixing liquid described in one side whipping step a) is while add urea and polyvinylpyrrolidone so that lanthanum nitrate
With being 1 with the mol ratio of polyvinylpyrrolidone:0.4, lanthanum nitrate is obtained with being 1 with the mol ratio of urea:2.8;Then by alleged by
The urea and polyvinylpyrrolidone taken is dissolved in mixed solution and stirs to clarify liquid;
C) clarified solution described in step b) is transferred to after being reacted 48 hours at 190 DEG C in 30ml high-temperature high-pressure reaction kettles
Obtain the dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder of triangle.
Gained triangle dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder through X-ray powder diffraction, ESEM identification with
And Room temperature PL spectrum (the dendritic europium doping lanthanum hydroxycarbonate of triangle prepared with embodiment 1 is similar), it is known that it is europium doping three
The dendritic lanthanum hydroxycarbonate in angle.
Embodiment 5
The preparation of the dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder of triangle, comprises the following steps:
A) appropriate lanthanum nitrate and the europium nitrate stirring and dissolving in the mixed solution of water and diglycol are weighed respectively, are made
It is 1 that lanthanum nitrate, which is obtained, with europium nitrate mol ratio:0.1, the volume ratio of water and diglycol is 1:1.2, then it will be weighed
Lanthanum nitrate and europium nitrate are dissolved in the mixed solution of water and diglycol;
B) mixing liquid described in one side whipping step a) is while add urea and polyvinylpyrrolidone so that lanthanum nitrate
With being 1 with the mol ratio of polyvinylpyrrolidone:0.5, lanthanum nitrate is obtained with being 1 with the mol ratio of urea:3.2;Then by alleged by
The urea and polyvinylpyrrolidone taken is dissolved in mixed solution and stirs to clarify liquid;
C) clarified solution described in step b) is transferred to after being reacted 36 hours at 170 DEG C in 30ml high-temperature high-pressure reaction kettles
Obtain the dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder of triangle.
Gained triangle dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder through X-ray powder diffraction, ESEM identification with
And Room temperature PL spectrum (the dendritic europium doping lanthanum hydroxycarbonate of triangle prepared with embodiment 1 is similar), it is known that it is that triangle is dendritic
Europium adulterates lanthanum hydroxycarbonate.
Embodiment 6
The preparation of the dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder of triangle, comprises the following steps:
A) appropriate lanthanum nitrate and the europium nitrate stirring and dissolving in the mixed solution of water and diglycol are weighed respectively, are made
It is 1 that lanthanum nitrate, which is obtained, with europium nitrate mol ratio:0.07, the volume ratio of water and diglycol is 1:1.5, then it will be weighed
Lanthanum nitrate and europium nitrate are dissolved in the mixed solution of water and diglycol;
B) mixing liquid described in one side whipping step a) is while add urea and polyvinylpyrrolidone so that lanthanum nitrate
With being 1 with the mol ratio of polyvinylpyrrolidone:0.4, lanthanum nitrate is obtained with being 3.5 with the mol ratio of urea;Then will be weighed
Urea and polyvinylpyrrolidone be dissolved in mixed solution and stir to clarify liquid;
C) clarified solution described in step b) is transferred to after being reacted 60 hours at 160 DEG C in 30ml high-temperature high-pressure reaction kettles
Obtain the dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder of triangle.
Gained triangle dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder through X-ray powder diffraction, ESEM identification with
And Room temperature PL spectrum (the dendritic europium doping lanthanum hydroxycarbonate of triangle prepared with embodiment 1 is similar), it is known that it is that triangle is dendritic
Europium adulterates lanthanum hydroxycarbonate.
Embodiment 7
The preparation of the dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder of triangle, comprises the following steps:
A) appropriate lanthanum nitrate and the europium nitrate stirring and dissolving in the mixed solution of water and diglycol are weighed respectively, are made
It is 1 that lanthanum nitrate, which is obtained, with europium nitrate mol ratio:0.06, the volume ratio of water and diglycol is 1:1, the nitre that then will be weighed
Sour lanthanum and europium nitrate are dissolved in the mixed solution of water and diglycol;
B) mixing liquid described in one side whipping step a) is while add urea and polyvinylpyrrolidone so that lanthanum nitrate
With being 1 with the mol ratio of polyvinylpyrrolidone:0.5, lanthanum nitrate is obtained with being 1 with the mol ratio of urea:2.3;Then by alleged by
The urea and polyvinylpyrrolidone taken is dissolved in mixed solution and stirs to clarify liquid;
C) clarified solution described in step b) is transferred to after being reacted 24 hours at 200 DEG C in 30ml high-temperature high-pressure reaction kettles
Obtain the dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder of triangle.
Gained triangle dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder through X-ray powder diffraction, ESEM identification with
And Room temperature PL spectrum (the dendritic europium doping lanthanum hydroxycarbonate of triangle prepared with embodiment 1 is similar), it is known that it is that triangle is dendritic
Europium adulterates lanthanum hydroxycarbonate.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than the present invention is protected
The limitation of scope is protected, although being explained in detail with reference to preferred embodiment to the present invention, one of ordinary skill in the art should
Understand, technical scheme can be modified or equivalent substitution, without departing from the essence of technical solution of the present invention
And scope.
Claims (5)
- A kind of 1. preparation method of the dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder of triangle, it is characterised in that methods described bag Include following steps:A) lanthanum salt and rare-earth europium salt are dissolved in mixed solution and the stirring of diglycol and water, the lanthanum salt and rare-earth europium gold The mol ratio for belonging to salt is 1:X, wherein 0<x<0.17;The volume ratio of water and diglycol is 1:Y, wherein 0.1<y<2;B) mixed solution described in one side whipping step a) is while add urea and polyvinylpyrrolidone, until urea and poly- second Alkene pyrrolidone is completely dissolved, and mixed liquor is clarified solution;C) clarified solution described in step b) is transferred under autoclave and reacted, reaction obtains the dendritic europium doping hydroxyl of triangle after terminating Base lanthanum carbonate red fluorescence powder;The lanthanum salt and the mol ratio of polyvinylpyrrolidone are 1:0.1~1:1;The lanthanum salt and the mol ratio of urea are 1:2~1:4.
- 2. the preparation method of the dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder of triangle according to claim 1, its feature It is:The rare-earth europium salt is one kind in europium nitrate or Europium chloride.
- 3. the preparation method of the dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder of triangle according to claim 1, its feature It is:The lanthanum salt is at least one of lanthanum nitrate, lanthanum chloride, lanthanum sulfate, lanthanum acetate.
- 4. the preparation method of the dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder of triangle according to claim 1, its feature It is:The volume ratio of the water and diglycol is 1:0.5~1:1.5.
- 5. the preparation method of the dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder of triangle according to claim 1, its feature It is:Step c) the mesohigh reactors volume is 30mL~50mL, and hydrothermal temperature is at 140~200 DEG C, the reaction time For 12h~72h.
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