CN106010539A - Blue light excited praseodymium doped lanthanum fluoride red-light phosphor and preparation method thereof - Google Patents
Blue light excited praseodymium doped lanthanum fluoride red-light phosphor and preparation method thereof Download PDFInfo
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- CN106010539A CN106010539A CN201610420348.5A CN201610420348A CN106010539A CN 106010539 A CN106010539 A CN 106010539A CN 201610420348 A CN201610420348 A CN 201610420348A CN 106010539 A CN106010539 A CN 106010539A
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- praseodymium
- doped lanthanum
- lanthanum fluoride
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/50—Wavelength conversion elements
- H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
- H01L33/502—Wavelength conversion materials
Abstract
The invention discloses a blue light excited praseodymium doped lanthanum fluoride red-light phosphor and a preparation method thereof. The chemical formula of the red-light phosphor is La[l-x]PrxF3, wherein x is larger than or equal to 10<-3> and smaller than or equal to 10<-1>, La[l-x]PrxF3 is praseodymium doped lanthanum fluoride powder, and the particle size ranges from 20 nm to 70 nm; the method comprises the steps that according to the components of La[l-x]PrxF3, a corresponding amount of lanthanum oxide, a corresponding amount of praseodymium oxide and an aqueous solution of nitric acid are prepared into an aqueous solution of rare earth nitrate under stirring, wherein the total rare earth ion concentration ranges from 0.1 mol/L to 0.5 mol/L; ammonium fluoride is added into the aqueous solution of rare earth nitrate for stirring, and a precursor solution is obtained; the precursor solution is placed in a closed state for reacting, and a reaction solution is obtained; the cooled reaction solution is subjected to solid-liquid separation, washing and drying in sequence, and the target product is obtained. The phosphor can be excited by blue light to emit red light, and the blue light excited praseodymium doped lanthanum fluoride red-light phosphor, a blue-light LED and a yellow-light phosphor can together be widely applied to indoor illumination of an LED easily.
Description
Technical field
The present invention relates to a kind of red light fluorescent powder and preparation method, a kind of blue light activated praseodymium doped lanthanum fluoride HONGGUANG is glimmering
Light powder and preparation method thereof.
Background technology
White light emitting diode (LED) has that volume is little, caloric value is low, less energy consumption, life-span length, reliability are high, pollution-free
Etc. advantage, it is described as the forth generation lighting source being to surmount electric filament lamp, fluorescent lamp and high intensity discharge etc..Along with white light
The application of LED constantly extends, and the requirement to its optical parametric is more and more higher, wherein it is important that light source is wanted
Ask closer to natural light.At present, the mode using LED to generate white light predominantly uses blue-ray LED to excite yellow fluorescent powder,
The gold-tinted synthesis white light sent by LED blue light and fluorescent material；Although this mode light efficiency is high, but because it lacks red spectrum
Point, cause that device color rendering index is relatively low, colour temperature is higher, significantly limit LED application in terms of room lighting.To this end,
People have made some good tries and effort, such as entitled " Color Kinetic Nanoparticles ",
J.Am.Chem.Soc., 2008,130,12222-12223 (" the color kinetic energy mechanics of nanoparticle ", " American Chemical Societies "
2008 volume 130 page 12222～12223) article.The red light fluorescent powder mentioned in this article is europium doping lanthanum fluoride
(LaF3: Eu3+) powder body, though it can be excited to send HONGGUANG, so need the black light using wavelength to be 250～400nm
Exciting, this just cannot only use blue-ray LED excitated fluorescent powder, to obtain the gold-tinted that sent by LED blue light and fluorescent material and red
Light synthesizes the white light being similar to nature light.
Summary of the invention
The technical problem to be solved in the present invention is for overcoming weak point of the prior art, it is provided that one is mixed by blue light activated praseodymium
Miscellaneous lanthanum fluoride red light fluorescent powder.
Another technical problem that the invention solves the problems that is for providing a kind of above-mentioned indigo plant light activated praseodymium doped lanthanum fluoride red light fluorescent powder
Preparation method.
For solving the technical problem of the present invention, the technical scheme used is: blue light activated praseodymium doped lanthanum fluoride HONGGUANG fluorescence
Powder includes having LaF3The fluorination lanthanio of chemical formula composition, particularly,
Chemical formula after described lanthanum fluoride is base and doped consists of La1-xPrxF3, in chemical formula 10-3≤x≤10-1；
Described La1-xPrxF3For powder body, described powder body is graininess, and the particle diameter of described granule is 20～70nm；
Described graininess La1-xPrxF3For praseodymium doped lanthanum fluoride.
Further improvement as blue light activated praseodymium doped lanthanum fluoride red light fluorescent powder:
Preferably, granule is tetragon, or hexagon.
For solving another technical problem of the present invention, another technical scheme used is: the light activated praseodymium of above-mentioned indigo plant is mixed
The preparation method of miscellaneous lanthanum fluoride red light fluorescent powder includes hydrothermal synthesis method, and particularly key step is as follows:
Step 1, first according to La1-xPrxF3Composition than weighing the lanthana (La of respective amount2O3) and praseodymium oxide (Pr2O3After),
The aqueous solution of nitric acid of lanthana, praseodymium oxide and 6～15mol/L is configured to stirring total rare earth (TRE) ion concentration be 0.1～
The rare earth nitrate aqueous solution of 0.5mol/L, then by ammonium fluoride (NH4F) adding in rare earth nitrate aqueous solution, stirring is to it
Reaction completely, obtains precursor solution, wherein, total rare earth (TRE) ion in precursor solution and the mol ratio of ammonium fluoride be 1:3～
4；
Step 2, is first placed in air-tight state by precursor solution, reacts at least 8h, obtain reactant liquor at 140～220 DEG C,
Chilled reactant liquor is carried out successively solid-liquid separation, the process washed and be dried again, prepares the fluorination of blue light activated praseodymium doped
Lanthanum red light fluorescent powder.
Further improvement as the preparation method of blue light activated praseodymium doped lanthanum fluoride red light fluorescent powder:
Preferably, solid-liquid separation is processed as centrifugation, and its rotating speed is 8000～12000r/min, the time is 5～15min.
Preferably, carrying out washing treatment is to use deionized water and ethanol that the solids of isolated carries out 2～3 times the most clear
Washing, separating solids during cleaning is centrifugation.
Preferably, dried is that the solids after cleaning is placed at 60～100 DEG C drying.
Provide the benefit that relative to prior art:
One, uses X-ray diffractometer, transmission electron microscope and steady-state lifetime fluorescence spectrophotometer to enter prepared purpose product respectively
Row characterizes, and from its result, the chemical formula of purpose product consists of La1-xPrxF3, in chemical formula 10-3≤x≤10-1；
Wherein, La1-xPrxF3For powder body, this powder body is the graininess of particle diameter 20～70nm, and granule is tetragon, or hexagon.?
Granular La1-xPrxF3For praseodymium doped lanthanum fluoride.Praseodymium doped lanthanum fluoride is excited by blue light and have issued HONGGUANG.
Its two, preparation method science, effectively.Not only prepare and mixed by the blue light activated praseodymium of blue light activated purpose product
Miscellaneous lanthanum fluoride red light fluorescent powder, also makes it compensate for blue-ray LED after being excited by blue light and excites yellow fluorescent powder to obtain white light LEDs
The red light portion of middle disappearance, more has the feature of low cost；And then make purpose product together with blue-ray LED and yellow fluorescent powder
It is extremely easy to be widely used in LED in indoor illumination.
Accompanying drawing explanation
Fig. 1 is to one of result that the purpose product that preparation method is prepared uses X-ray diffraction (XRD) instrument to characterize.XRD
Spectrogram shows that purpose product is praseodymium doping lanthanum fluoride (La1-xPrxF3)。
Fig. 2 is to one of result that prepared purpose product use transmission electron microscope (TEM) characterizes.TEM image demonstrates
Purpose product is nano level particulate matter.
Fig. 3 is to one of result that prepared purpose product use steady-state lifetime fluorescence spectrophotometer characterizes.Its result confirms
Purpose product 440～480nm blue light excite under have issued HONGGUANG.
Detailed description of the invention
Below in conjunction with the accompanying drawings the optimal way of the present invention is described in further detail.
First buy from market or prepare voluntarily:
Lanthana；Praseodymium oxide；Aqueous solution of nitric acid；Ammonium fluoride.
Then,
Embodiment 1
Concretely comprising the following steps of preparation:
Step 1, first according to La0.999Pr0.001F3Composition than weighing lanthana and the praseodymium oxide of respective amount after, by lanthana, oxygen
The aqueous solution of nitric acid changing praseodymium and 6mol/L is configured to the rare earth nitrate water that total rare earth (TRE) ion concentration is 0.1mol/L with stirring
Solution.Again ammonium fluoride is added in rare earth nitrate aqueous solution, stir to its reaction completely, obtain precursor solution；Wherein,
Total rare earth (TRE) ion and the mol ratio of ammonium fluoride in precursor solution are 1:3.
Step 2, is first placed in air-tight state by precursor solution, reacts 24h, obtain reactant liquor at 140 DEG C.Again to cooling
Reactant liquor carry out solid-liquid separation, the process washed and be dried successively；Wherein, solid-liquid separation is processed as centrifugation, its
Rotating speed is 8000r/min, the time is 15min, and carrying out washing treatment is to use deionized water and ethanol to enter the solids of isolated
The alternately cleaning that row is 2 times, separating solids during cleaning is centrifugation, and dried is that the solids after cleaning is placed in 60 DEG C
Lower drying.Prepare and be similar to Fig. 2, and the indigo plant light activated praseodymium doped lanthanum fluoride as shown in the curve in Fig. 1 and Fig. 3 is red
Emitting phosphor.
Embodiment 2
Concretely comprising the following steps of preparation:
Step 1, first according to La0.995Pr0.005F3Composition than weighing lanthana and the praseodymium oxide of respective amount after, by lanthana, oxygen
The aqueous solution of nitric acid changing praseodymium and 9mol/L is configured to the rare earth nitrate water that total rare earth (TRE) ion concentration is 0.2mol/L with stirring
Solution.Again ammonium fluoride is added in rare earth nitrate aqueous solution, stir to its reaction completely, obtain precursor solution；Wherein,
Total rare earth (TRE) ion and the mol ratio of ammonium fluoride in precursor solution are 1:3.3.
Step 2, is first placed in air-tight state by precursor solution, reacts 20h, obtain reactant liquor at 160 DEG C.Again to cooling
Reactant liquor carry out solid-liquid separation, the process washed and be dried successively；Wherein, solid-liquid separation is processed as centrifugation, its
Rotating speed is 9000r/min, the time is 13min, and carrying out washing treatment is to use deionized water and ethanol to enter the solids of isolated
The alternately cleaning that row is 2 times, separating solids during cleaning is centrifugation, and dried is that the solids after cleaning is placed in 70 DEG C
Lower drying.Prepare and be similar to Fig. 2, and the indigo plant light activated praseodymium doped lanthanum fluoride as shown in the curve in Fig. 1 and Fig. 3 is red
Emitting phosphor.
Embodiment 3
Concretely comprising the following steps of preparation:
Step 1, first according to La0.99Pr0.01F3Composition than weighing lanthana and the praseodymium oxide of respective amount after, by lanthana, oxygen
The aqueous solution of nitric acid changing praseodymium and 11mol/L is configured to the rare earth nitrate water that total rare earth (TRE) ion concentration is 0.3mol/L with stirring
Solution.Again ammonium fluoride is added in rare earth nitrate aqueous solution, stir to its reaction completely, obtain precursor solution；Wherein,
Total rare earth (TRE) ion and the mol ratio of ammonium fluoride in precursor solution are 1:3.5.
Step 2, is first placed in air-tight state by precursor solution, reacts 16h, obtain reactant liquor at 180 DEG C.Again to cooling
Reactant liquor carry out solid-liquid separation, the process washed and be dried successively；Wherein, solid-liquid separation is processed as centrifugation, its
Rotating speed is 10000r/min, the time is 10min, and carrying out washing treatment is to use deionized water and the ethanol solids to isolated
Carrying out the alternately cleaning of 3 times, separating solids during cleaning is centrifugation, and dried is that the solids after cleaning is placed in
Dry at 80 DEG C.Prepare such as Fig. 2, and the indigo plant light activated praseodymium doped lanthanum fluoride as shown in the curve in Fig. 1 and Fig. 3 is red
Emitting phosphor.
Embodiment 4
Concretely comprising the following steps of preparation:
Step 1, first according to La0.95Pr0.05F3Composition than weighing lanthana and the praseodymium oxide of respective amount after, by lanthana, oxygen
The aqueous solution of nitric acid changing praseodymium and 13mol/L is configured to the rare earth nitrate water that total rare earth (TRE) ion concentration is 0.4mol/L with stirring
Solution.Again ammonium fluoride is added in rare earth nitrate aqueous solution, stir to its reaction completely, obtain precursor solution；Wherein,
Total rare earth (TRE) ion and the mol ratio of ammonium fluoride in precursor solution are 1:3.8.
Step 2, is first placed in air-tight state by precursor solution, reacts 12h, obtain reactant liquor at 200 DEG C.Again to cooling
Reactant liquor carry out solid-liquid separation, the process washed and be dried successively；Wherein, solid-liquid separation is processed as centrifugation, its
Rotating speed is 11000r/min, the time is 8min, and carrying out washing treatment is to use deionized water and ethanol to enter the solids of isolated
The alternately cleaning that row is 3 times, separating solids during cleaning is centrifugation, and dried is that the solids after cleaning is placed in 90 DEG C
Lower drying.Prepare and be similar to Fig. 2, and the indigo plant light activated praseodymium doped lanthanum fluoride as shown in the curve in Fig. 1 and Fig. 3 is red
Emitting phosphor.
Embodiment 5
Concretely comprising the following steps of preparation:
Step 1, first according to La0.9Pr0.1F3Composition than weighing lanthana and the praseodymium oxide of respective amount after, by lanthana, oxidation
It is water-soluble that the aqueous solution of nitric acid of praseodymium and 15mol/L is configured to the rare earth nitrate that total rare earth (TRE) ion concentration is 0.5mol/L with stirring
Liquid.Again ammonium fluoride is added in rare earth nitrate aqueous solution, stir to its reaction completely, obtain precursor solution；Wherein,
Total rare earth (TRE) ion and the mol ratio of ammonium fluoride in precursor solution are 1:4.
Step 2, is first placed in air-tight state by precursor solution, reacts 8h, obtain reactant liquor at 220 DEG C.Again to cooling
Reactant liquor carry out solid-liquid separation, the process washed and be dried successively；Wherein, solid-liquid separation is processed as centrifugation, its
Rotating speed is 12000r/min, the time is 5min, and carrying out washing treatment is to use deionized water and ethanol to enter the solids of isolated
The alternately cleaning that row is 3 times, separating solids during cleaning is centrifugation, and dried is that the solids after cleaning is placed in
Dry at 100 DEG C.Prepare and be similar to Fig. 2, and the indigo plant light activated praseodymium doped fluorination as shown in the curve in Fig. 1 and Fig. 3
Lanthanum red light fluorescent powder.
Obviously, those skilled in the art can praseodymium doped lanthanum fluoride red light fluorescent powder light activated to the indigo plant of the present invention and system thereof
Preparation Method carries out various change and modification without departing from the spirit and scope of the present invention.So, if these of the present invention are repaiied
Change and belong within the scope of the claims in the present invention and equivalent technologies thereof with modification, then the present invention be also intended to comprise these change and
Including modification.
Claims (6)
1. an indigo plant light activated praseodymium doped lanthanum fluoride red light fluorescent powder, including having LaF3The fluorination lanthanio of chemical formula composition,
It is characterized in that:
Chemical formula after described lanthanum fluoride is base and doped consists of La1-xPrxF3, in chemical formula 10-3≤x≤10-1；
Described La1-xPrxF3For powder body, described powder body is graininess, and the particle diameter of described granule is 20～70nm；
Described graininess La1-xPrxF3For praseodymium doped lanthanum fluoride.
Indigo plant the most according to claim 1 light activated praseodymium doped lanthanum fluoride red light fluorescent powder, is characterized in that granule is four limits
Shape, or hexagon.
3. a preparation method for blue light activated praseodymium doped lanthanum fluoride red light fluorescent powder described in claim 1, closes including hydro-thermal
Cheng Fa, it is characterised in that key step is as follows:
Step 1, first according to La1-xPrxF3Composition than weighing lanthana and the praseodymium oxide of respective amount after, by lanthana, oxidation
Praseodymium and 6～15mol/L aqueous solution of nitric acid be configured to the rare earth nitre that total rare earth (TRE) ion concentration is 0.1～0.5mol/L with stirring
Acid salt aqueous solution, then ammonium fluoride is added in rare earth nitrate aqueous solution, stir to its reaction completely, obtain precursor solution,
Wherein, the mol ratio of the total rare earth (TRE) ion in precursor solution and ammonium fluoride is 1:3～4；
Step 2, is first placed in air-tight state by precursor solution, reacts at least 8h, obtain reactant liquor at 140～220 DEG C,
Chilled reactant liquor is carried out successively solid-liquid separation, the process washed and be dried again, prepares the fluorination of blue light activated praseodymium doped
Lanthanum red light fluorescent powder.
The preparation method of indigo plant the most according to claim 3 light activated praseodymium doped lanthanum fluoride red light fluorescent powder, is characterized in that
Solid-liquid separation is processed as centrifugation, and its rotating speed is 8000～12000r/min, the time is 5～15min.
The preparation method of indigo plant the most according to claim 3 light activated praseodymium doped lanthanum fluoride red light fluorescent powder, is characterized in that
Carrying out washing treatment is the alternately cleaning using deionized water and ethanol that the solids of isolated carries out 2～3 times, separates during cleaning
Solids is centrifugation.
The preparation method of indigo plant the most according to claim 3 light activated praseodymium doped lanthanum fluoride red light fluorescent powder, is characterized in that
Dried is that the solids after cleaning is placed at 60～100 DEG C drying.
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| WO2006113998A1 (en) * | 2005-04-26 | 2006-11-02 | University Of Victoria Innovation And Development Corporation | Production of light from sol-gel derived thin films made with lanthanide doped nanoparticles, and preparation thereof |
| CN102676171A (en) * | 2011-03-14 | 2012-09-19 | 中国科学院福建物质结构研究所 | Method for synthesizing amino functionalized rare earth-doped lanthanum fluoride nano fluorescent marker material |
| CN103571491A (en) * | 2012-07-27 | 2014-02-12 | 海洋王照明科技股份有限公司 | Praseodymium-holmium-codoped lanthanum fluoride up-conversion luminescence material, and preparation method and application thereof |
-
2016
- 2016-06-07 CN CN201610420348.5A patent/CN106010539A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006113998A1 (en) * | 2005-04-26 | 2006-11-02 | University Of Victoria Innovation And Development Corporation | Production of light from sol-gel derived thin films made with lanthanide doped nanoparticles, and preparation thereof |
| CN102676171A (en) * | 2011-03-14 | 2012-09-19 | 中国科学院福建物质结构研究所 | Method for synthesizing amino functionalized rare earth-doped lanthanum fluoride nano fluorescent marker material |
| CN103571491A (en) * | 2012-07-27 | 2014-02-12 | 海洋王照明科技股份有限公司 | Praseodymium-holmium-codoped lanthanum fluoride up-conversion luminescence material, and preparation method and application thereof |
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| W.J.SCHIPPER,等: "On the recombination mechanism in X-ray storage phosphors based on lanthanum fluoride", 《JOURNAL OF LUMINESCENCE》 * |
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