CN104592994A - Preparation method of triangular dendritic europium-doped lanthanum hydroxycarbonate red fluorescent powder - Google Patents
Preparation method of triangular dendritic europium-doped lanthanum hydroxycarbonate red fluorescent powder Download PDFInfo
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- CN104592994A CN104592994A CN201510018928.7A CN201510018928A CN104592994A CN 104592994 A CN104592994 A CN 104592994A CN 201510018928 A CN201510018928 A CN 201510018928A CN 104592994 A CN104592994 A CN 104592994A
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Abstract
The invention discloses a preparation method of triangular dendritic europium-doped lanthanum hydroxycarbonate red fluorescent powder, which comprises the following steps: a) dissolving lanthanum salt and rare-earth europium salt in a diglycol-water mixed liquid, and stirring; b) adding urea and polyvinylpyrrolidone into the mixed liquid in the step a) while stirring until the urea is completely dissolved, thereby obtaining a colorless transparent liquid; and c) transferring the colorless transparent liquid in the step b) into a high-pressure reaction kettle, and reacting to obtain the europium-doped triangular dendritic lanthanum hydroxycarbonate. The method has the advantages of low raw material cost, simple synthesis technique, stable product quality, favorable technical repetitiveness and strong red light emission of the product, and can implement large-scale industrialization. The product prepared by the method can be widely used in the fields of agricultural film optical transfer agents, fluorescent powder for PDP (plasma display panel) and LED (light-emitting diode), and other high technologies.
Description
Technical field
The present invention relates to red light electroluminescent material field, particularly the preparation method of a kind of triangle dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder.
Background technology
Agricultural is the basis of the national economy of China, improves the sound development that Crop yield and quality can promote China's economy further.Compare with the external conditions such as fertilising with cultivating of farm crop, wherein light conversion film technology promotes that farm crop make full use of the sun and strengthen photosynthesis, has not only had an economic benefit but also have environment protection significance.Especially light-converting film high energy UV being converted into the blood orange light of photosynthesis of plant gains great popularity.The rare earth inorganic fluorescent material light-converting agent of current optical transfer agricultural film can convert UV-light to blood orange light, and production cost is lower, and has stronger luminescent properties and ageing-resistant function.
The factor affecting light-emitting phosphor efficiency comprises the particle diameter and pattern etc. thereof of the crystalline structure of matrix, the doping content of rare earth ion and distribution thereof, luminescent material.Therefore, the luminescence center selecting luminescence strong and the good luminous host of optical property particularly important.Europium ion has stronger red emission at about 620nm, is often selected as the luminescence center of red fluorescence material; In addition, because lanthanum hydroxycarbonate possesses six good side's phase crystalline structure and physicalies, be also often selected as the luminous host of red fluorescence material and prepare the presoma of lanthanum hydroxide and lanthanum trioxide, and passing through forerunner La (CO)
3the thermal treatment of OH, can obtain La (OH) more stable on thermodynamics
3and La
2o
3.So far, rear-earth-doped La (CO)
3oH fluorescent material adopts the preparations such as the precipitator method, sol-gel method, template-directing method, microemulsion method and hydrothermal method usually, and gained sample majority is six side's phase structures.Therefore, for obtaining the more excellent red fluorescence material of optical property, that seeks a kind of simple and easy preparation six side phase mixes europium La (CO)
3the method of OH seems particularly crucial.
In recent years, along with the development of farming technology, various agricultural functional material more and more to low cost and high-quality future development, puts forward higher requirement to function agricultural material.Doping vario-property becomes and improves rear-earth-doped La (CO)
3a kind of effective means of OH device for Optical Properties of Materials.Mix europium La (CO)
3the particle diameter of OH red fluorescence material, pattern, chemical constitution and dispersion of particles state etc. all have a strong impact on its optical property and physicals and the application in optical transfer agricultural film.Therefore, the breakthrough point that granule regularizing triangle dendritic europium doping lanthanum hydroxycarbonate fluorescent material is also prior art how is synthesized.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art and provide that a kind of low in raw material price, target product are controlled, preparation technology is simple, there is good red emission and be easy to industrial red fluorescence powder, preparation method thereof.
For achieving the above object, the technical scheme that the present invention takes is: the preparation method of a kind of triangle dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder, comprises the following steps:
A) lanthanum salt and rare-earth europium salt are dissolved in the mixing solutions of glycol ether and water and stir, the mol ratio of described lanthanum salt and rare-earth europium metal-salt is 1:x, wherein 0<x<0.1; The volume ratio of water and glycol ether is 1:y, wherein 0.1<y<2;
B) on one side whipping step a) described in mixing liquid while add urea and polyvinylpyrrolidone, until urea dissolves completely obtain colourless transparent liquid;
C) by step b) described in colourless transparent liquid to be transferred under autoclave in reaction, obtain linen triangle dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder.
As the preferred implementation of the preparation method of triangle of the present invention dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder, described europium metal-salt is the one in europium nitrate or corresponding muriate.
As the preferred implementation of the preparation method of triangle of the present invention dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder, described lanthanum salt is at least one in lanthanum nitrate, Lanthanum trichloride, lanthanum sulfat, lanthanum acetate.
As the preferred implementation of the preparation method of triangle of the present invention dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder, the volume ratio of described water and glycol ether is 1:0.5 ~ 1:1.5.
As the preferred implementation of the preparation method of triangle of the present invention dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder, the mol ratio of described lanthanum salt and polyvinylpyrrolidone is 1:0.1 ~ 1:1.
As the preferred implementation of the preparation method of triangle of the present invention dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder, the mol ratio of described lanthanum salt and urea is 1:2 ~ 1:4.
As the preferred implementation of the preparation method of triangle of the present invention dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder, described step c) mesohigh reactor volume is 30ml, hydrothermal temperature is at 140 DEG C ~ 200 DEG C, and the reaction times is 12h ~ 72h.
In invention, polyvinylpyrrolidone dissolves in the solution as a kind of soft mode version, in lanthanum hydroxycarbonate process of growth, be adsorbed on its anisotropic growth of lanthanum hydroxycarbonate spatial induction, finally make to mix europium lanthanum hydroxycarbonate and self-assembly can form triangle branched structure.
The preparation method of a kind of triangle of the present invention dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder, has following beneficial effect:
(1) cheaper starting materials of preparation method provided by the invention is easy to get, and cost is low, and synthesis technique is simple and easy to realize, and constant product quality and process repeatability can be good;
(2) the 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 described method can be widely used in agricultural film light-converting agent, PDP, LED fluorescent material and other high-tech area.
Accompanying drawing explanation
The X-ray diffractogram of the triangle of Fig. 1 prepared by embodiments of the invention 1 dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder.
The scanning electron microscope (SEM) photograph of the triangle of Fig. 2 prepared by embodiments of the invention 1 dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder.
The room temperature absorption spectra of the triangle of Fig. 3 prepared by embodiments of the invention 1 dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder.
Embodiment
For better the object, technical solutions and advantages of the present invention being described, below in conjunction with the drawings and specific embodiments, the invention will be further described.
Embodiment 1
The preparation of triangle dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder, comprises the following steps:
A) appropriate lanthanum nitrate and europium nitrate stirring and dissolving in the mixing solutions of water and glycol ether is taken respectively, lanthanum nitrate and europium nitrate mol ratio is made to be 1:0.05, the volume ratio of water and glycol ether is 1:0.8, then by taken lanthanum nitrate and the water-soluble mixing solutions with glycol ether of europium nitrate;
B) on one side whipping step a) described in mixing liquid while add urea and polyvinylpyrrolidone, the mol ratio making lanthanum nitrate and polyvinylpyrrolidone is 1:0.3, and the mol ratio obtaining lanthanum nitrate and urea is 1:2; Then taken urea and polyvinylpyrrolidone be dissolved in mixing solutions and stir to clarify liquid;
C) by step b) described in clear liquor transfer in 30ml high-temperature high-pressure reaction kettle to react at 180 DEG C after 24 hours and obtain triangle dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder.
Gained triangle dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder is accredited as six side's phase lanthanum hydroxycarbonates through X-ray powder diffraction, and powder x-ray diffraction result as shown in Figure 1; Material morphology is obtained by scanning electron microscope result, as shown in Figure 2.As Fig. 2 can find out that material granule is regular, particle is triangle branched structure; Fig. 3 is the Room temperature PL spectrum of this sample, and triangle dendritic europium doping lanthanum hydroxycarbonate excites in 262nm wavelength light has emission peak at 593nm, 619nm, 650nm and 793nm place respectively down, and red luminous intensity is maximum at 619nm place.
Embodiment 2
The preparation of triangle dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder, comprises the following steps:
A) taking appropriate lanthanum nitrate and europium nitrate respectively in the mixing solutions of water and glycol ether stirs, lanthanum nitrate and europium nitrate mol ratio is made to be 1:0.08, the volume ratio of water and glycol ether is 1:1, then by taken lanthanum nitrate and the water-soluble mixing solutions with glycol ether of europium nitrate;
B) on one side whipping step a) described in mixing liquid while add urea and polyvinylpyrrolidone, make lanthanum nitrate and be 1:0.5 with the mol ratio of polyvinylpyrrolidone, obtain lanthanum nitrate and be 1:3 with the mol ratio of urea; Then taken urea and polyvinylpyrrolidone be dissolved in mixing solutions and stir to clarify liquid;
C) by step b) described in clear liquor transfer in 30ml high-temperature high-pressure reaction kettle to react at 190 DEG C after 24 hours and obtain the dendritic lanthanum hydroxycarbonate red fluorescence powder of europium doping triangle.
Gained triangle dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder is through X-ray powder diffraction, scanning electron microscope qualification and Room temperature PL spectrum (the triangle dendritic europium doping lanthanum hydroxycarbonate prepared with embodiment 1 is similar), and known its is triangle dendritic europium doping lanthanum hydroxycarbonate.
Embodiment 3
The preparation of triangle dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder, comprises the following steps:
A) taking appropriate lanthanum nitrate and europium nitrate respectively in the mixing solutions of water and glycol ether stirs, lanthanum nitrate and europium nitrate mol ratio is made to be 1:0.09, the volume ratio of water and glycol ether is 1:0.5, then by taken lanthanum nitrate and the water-soluble mixing solutions with glycol ether of europium nitrate;
B) on one side whipping step a) described in mixing liquid while add urea and polyvinylpyrrolidone, make lanthanum nitrate and be 1:0.5 with the mol ratio of polyvinylpyrrolidone, obtain lanthanum nitrate and be 1:2.5 with the mol ratio of urea; Then taken urea and polyvinylpyrrolidone be dissolved in mixing solutions and stir to clarify liquid;
C) by step b) described in clear liquor transfer in 30ml high-temperature high-pressure reaction kettle to react at 180 DEG C after 48 hours and obtain triangle dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder.
Gained triangle dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder is through X-ray powder diffraction, scanning electron microscope qualification and Room temperature PL spectrum (the triangle dendritic europium doping lanthanum hydroxycarbonate prepared with embodiment 1 is similar), and known its is triangle dendritic europium doping lanthanum hydroxycarbonate.
Embodiment 4
The preparation of the dendritic lanthanum hydroxycarbonate red fluorescence powder of europium doping triangle, comprises the following steps:
A) appropriate lanthanum nitrate and europium nitrate stirring and dissolving in the mixing solutions of water and glycol ether is taken respectively, lanthanum nitrate and europium nitrate mol ratio is made to be 1:0.05, the volume ratio of water and glycol ether is 1:1.3, then by taken lanthanum nitrate and the water-soluble mixing solutions with glycol ether of europium nitrate;
B) on one side whipping step a) described in mixing liquid while add urea and polyvinylpyrrolidone, make lanthanum nitrate and be 1:0.4 with the mol ratio of polyvinylpyrrolidone, obtain lanthanum nitrate and be 1:2.8 with the mol ratio of urea; Then taken urea and polyvinylpyrrolidone be dissolved in mixing solutions and stir to clarify liquid;
C) by step b) described in clear liquor transfer in 30ml high-temperature high-pressure reaction kettle to react at 190 DEG C after 48 hours and obtain triangle dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder.
Gained triangle dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder is through X-ray powder diffraction, scanning electron microscope qualification and Room temperature PL spectrum (the triangle dendritic europium doping lanthanum hydroxycarbonate prepared with embodiment 1 is similar), and known its is the dendritic lanthanum hydroxycarbonate of europium doping triangle.
Embodiment 5
The preparation of triangle dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder, comprises the following steps:
A) appropriate lanthanum nitrate and europium nitrate stirring and dissolving in the mixing solutions of water and glycol ether is taken respectively, lanthanum nitrate and europium nitrate mol ratio is made to be 1:0.1, the volume ratio of water and glycol ether is 1:1.2, then by taken lanthanum nitrate and the water-soluble mixing solutions with glycol ether of europium nitrate;
B) on one side whipping step a) described in mixing liquid while add urea and polyvinylpyrrolidone, make lanthanum nitrate and be 1:0.5 with the mol ratio of polyvinylpyrrolidone, obtain lanthanum nitrate and be 1:3.2 with the mol ratio of urea; Then taken urea and polyvinylpyrrolidone be dissolved in mixing solutions and stir to clarify liquid;
C) by step b) described in clear liquor transfer in 30ml high-temperature high-pressure reaction kettle to react at 170 DEG C after 36 hours and obtain triangle dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder.
Gained triangle dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder is through X-ray powder diffraction, scanning electron microscope qualification and Room temperature PL spectrum (the triangle dendritic europium doping lanthanum hydroxycarbonate prepared with embodiment 1 is similar), and known its is triangle dendritic europium doping lanthanum hydroxycarbonate.
Embodiment 6
The preparation of triangle dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder, comprises the following steps:
A) appropriate lanthanum nitrate and europium nitrate stirring and dissolving in the mixing solutions of water and glycol ether is taken respectively, lanthanum nitrate and europium nitrate mol ratio is made to be 1:0.07, the volume ratio of water and glycol ether is 1:1.5, then by taken lanthanum nitrate and the water-soluble mixing solutions with glycol ether of europium nitrate;
B) on one side whipping step a) described in mixing liquid while add urea and polyvinylpyrrolidone, make lanthanum nitrate and be 1:0.4 with the mol ratio of polyvinylpyrrolidone, obtain lanthanum nitrate and be 3.5 with the mol ratio of urea; Then taken urea and polyvinylpyrrolidone be dissolved in mixing solutions and stir to clarify liquid;
C) by step b) described in clear liquor transfer in 30ml high-temperature high-pressure reaction kettle to react at 160 DEG C after 60 hours and obtain triangle dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder.
Gained triangle dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder is through X-ray powder diffraction, scanning electron microscope qualification and Room temperature PL spectrum (the triangle dendritic europium doping lanthanum hydroxycarbonate prepared with embodiment 1 is similar), and known its is triangle dendritic europium doping lanthanum hydroxycarbonate.
Embodiment 7
The preparation of triangle dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder, comprises the following steps:
A) appropriate lanthanum nitrate and europium nitrate stirring and dissolving in the mixing solutions of water and glycol ether is taken respectively, lanthanum nitrate and europium nitrate mol ratio is made to be 1:0.06, the volume ratio of water and glycol ether is 1:1, then by taken lanthanum nitrate and the water-soluble mixing solutions with glycol ether of europium nitrate;
B) on one side whipping step a) described in mixing liquid while add urea and polyvinylpyrrolidone, make lanthanum nitrate and be 1:0.5 with the mol ratio of polyvinylpyrrolidone, obtain lanthanum nitrate and be 1:2.3 with the mol ratio of urea; Then taken urea and polyvinylpyrrolidone be dissolved in mixing solutions and stir to clarify liquid;
C) by step b) described in clear liquor transfer in 30ml high-temperature high-pressure reaction kettle to react at 200 DEG C after 24 hours and obtain triangle dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder.
Gained triangle dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder is through X-ray powder diffraction, scanning electron microscope qualification and Room temperature PL spectrum (the triangle dendritic europium doping lanthanum hydroxycarbonate prepared with embodiment 1 is similar), and known its is triangle dendritic europium doping lanthanum hydroxycarbonate.
Finally to should be noted that; above embodiment is only in order to illustrate technical scheme of the present invention but not limiting the scope of the invention; although be explained in detail the present invention with reference to preferred embodiment; those of ordinary skill in the art is to be understood that; can modify to technical scheme of the present invention or equivalent replacement, and not depart from essence and the scope of technical solution of the present invention.
Claims (7)
1. a preparation method for triangle dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder, is characterized in that, said method comprising the steps of:
A) lanthanum salt and rare-earth europium salt are dissolved in the mixing solutions of glycol ether and water and stir, the mol ratio of described lanthanum salt and rare-earth europium metal-salt is 1:x, wherein 0<x<0.17; The volume ratio of water and glycol ether is 1:y, wherein 0.1<y<2;
B) on one side whipping step a) described in mixing solutions while add urea and polyvinylpyrrolidone, until urea and polyvinylpyrrolidone dissolve completely, mixed solution is clear liquor;
C) by step b) described in clear liquor proceed to autoclave under react, obtain triangle dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder after reaction terminates.
2. the preparation method of triangle according to claim 1 dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder, is characterized in that: described rare-earth europium salt is the one in europium nitrate or Europium trichloride.
3. the preparation method of triangle according to claim 1 dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder, is characterized in that: described lanthanum salt is at least one in lanthanum nitrate, Lanthanum trichloride, lanthanum sulfat, lanthanum acetate.
4. the preparation method of triangle according to claim 1 dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder, is characterized in that: the volume ratio of described water and glycol ether is 1:0.5 ~ 1:1.5.
5. the preparation method of triangle according to claim 1 dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder, is characterized in that: the mol ratio of described lanthanum salt and polyvinylpyrrolidone is 1:0.1 ~ 1:1.
6. the preparation method of triangle according to claim 1 dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder, is characterized in that: the mol ratio of described lanthanum salt and urea is 1:2 ~ 1:4.
7. the preparation method of triangle according to claim 1 dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder, it is characterized in that: described step c) mesohigh reactor volume is 30ml ~ 50ml, hydrothermal temperature is at 140 ~ 200 DEG C, and the reaction times is 12h ~ 72h.
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| CN109321250A (en) * | 2018-10-25 | 2019-02-12 | 惠州学院 | A kind of nanoscale lanthanum orthophosphate yttrium base red fluorescent powder and preparation method thereof |
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