CN109135743A - A kind of high-dopant concentration red fluorescence powder and preparation method thereof - Google Patents
A kind of high-dopant concentration red fluorescence powder and preparation method thereof Download PDFInfo
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- CN109135743A CN109135743A CN201810641884.7A CN201810641884A CN109135743A CN 109135743 A CN109135743 A CN 109135743A CN 201810641884 A CN201810641884 A CN 201810641884A CN 109135743 A CN109135743 A CN 109135743A
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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
- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
- C09K11/7784—Chalcogenides
- C09K11/7787—Oxides
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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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
- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
- C09K11/7794—Vanadates; Chromates; Molybdates; Tungstates
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Abstract
The present invention relates to phosphor material powder technical fields, in particular a kind of high-dopant concentration red fluorescence powder and preparation method thereof, the following steps are included: S1, it is raw material that the raw material for choosing manufacture high-dopant concentration red fluorescence powder, which include: wolframic acid ammonia (H40N10O41W12XH2O), lanthanum nitrate (La (NO3) 3nH2O) and europium nitrate (Eu (NO3) 3), and deionized water, ammonium hydroxide are solvent；S2, select tool include: electronic balance, key, beaker, glass bar, pipette, 150ml volumetric flask, water heating kettle, centrifuge tube, centrifuge, magnetic stir bar, blender, baking oven, grinding rod, PH test paper and mortar；S3, raw material are weighed: weighing the solid of La (NO3) 3nH2O and H40N10O41W12XH2O by upper table dosage requirement using electronic balance, a small amount of deionized water is added to dissolve in small beaker respectively, and be sufficiently stirred, form configured 3 solution of Eu (NO3) that mixed liquor pipettes specified amount with pipette again.Operation of the present invention step will not rigorously impact subsequent operation, while good fluorescent powder proportion has been obtained in high-dopant concentration.
Description
Technical field
The present invention relates to phosphor material powder technical field more particularly to a kind of high-dopant concentration red fluorescence powder and its preparations
Method.
Background technique
Currently, white light emitting diode W-LED (White Light Emitting Diode) is a kind of by turning electric energy
It is changed to the energy conversion device of luminous energy, the approach of whole realization is that fluorescent material is coated on luminous semiconductor chip, the fluorescence
Material passes through the excitation of semiconductor light emitting, can issue various fluorescence, the light and semiconductor chip intrinsic light of sending are blended in one
It rises, so as to obtain the light source of white light；White light emitting diode has low operating voltage, saving electricity, performance stable, device
Service life is long, vibration resistance is strong, integral device is light-weight and it is small in size, luminescence response is fast, coloration is adjustable the advantages that.Therefore exist
Display light source field rapidly develops W-LED and gradually replaces incandescent lamp and fluorescent lamp in lighting area.
After Ya company of Japan in 1993 successfully develops first efficient GaInN system blue-ray LED in the world, make
Full color LED is obtained to be achieved.High-luminous-efficiency and the performance of low-power consumption make LED have broad application prospects.In order to
It realizes white light LEDs (W-LED), currently more feasible method is to utilize light conversion phosphor method, still, quotient currently on the market
It is mainly 22 O of O 3:Eu 3+ and Y of Y, 2 S:Eu 3+ with rouge and powder, these fluorescent powders are mainly used to high-pressure sodium lamp (fluorescent lamp),
It is not to be developed near ultraviolet LED chip.Such as 22 O of O 3:Eu 3+ and Y of Y, 2 S:Eu 3+ fluorescent powder mainly forms
It is all that rare earth element is expensive, wherein there is also the problem of heat-resistant stability difference, prolonged uses by 2 O of Y, 2 S:Eu 3+
The phenomenon that will appear color drift, it is low (about 1%) to additionally, there may be its quenching concentration, therefore, find it is a kind of efficiently, stablize
LED is necessary with red fluorescence.
Therefore a kind of high-concentration dopant, high efficiency red phosphor powder are needed adapting to the development of society and are improved.
Summary of the invention
The purpose of the present invention is to solve disadvantages existing in the prior art, and propose.
To achieve the goals above, present invention employs following technical solutions:
A kind of high-dopant concentration red fluorescence powder and preparation method thereof, comprising the following steps:
S1, the raw material for choosing manufacture high-dopant concentration red fluorescence powder include: wolframic acid ammonia (H40N10O41W12
XH2O), lanthanum nitrate (La (NO3) 3nH2O) and europium nitrate (Eu (NO3) 3) are raw material, and deionized water, ammonium hydroxide are solvent.
S2, select tool include: electronic balance, key, beaker, glass bar, pipette, 150ml volumetric flask, water heating kettle,
Centrifuge tube, centrifuge, magnetic stir bar, blender, baking oven, grinding rod, PH test paper and mortar；
S3, to raw material weigh: using electronic balance by upper table dosage requirements weighing La (NO3) 3 nH2O with
The solid of H40N10O41W12XH2O adds a small amount of deionized water to dissolve in small beaker respectively, and is sufficiently stirred, and is formed
Mixed liquor pipettes configured 3 solution of Eu (NO3) of specified amount with pipette again, then suitably adds deionized water, uses ammonium hydroxide
It adjusts solution and is 9 or so with PH test paper test solution PH；It is put into magnetic stir bar in the solution, is stirred with magnetic stirrer；
The solution being stirred and precipitating are packed into water heating kettle together, add appropriate amount of deionized water, and solution is divided into 4 by S4
4 groups of samples are moved into baking oven together, set constant 180 DEG C, time 12h of the position of drying temperature, carry out hydro-thermal reaction by group；
S5 takes out and completes the sample of hydro-thermal reaction and be centrifuged, removes supernatant liquor, then with appropriate amount of deionized water by powder
Move into centrifuge tube；
4 groups of centrifuge tubes are uniformly put into drying 48h or more in 80 DEG C of -85 DEG C of baking ovens, take out centrifuge tube, ground with mortar by S6
Be milled body 5-10min, envelope；
S7 takes out envelope finished product and carries out fluorophor performance test.
Preferably, it is described weigh La (NO3) 3nH2O and H40N10O41W12XH2O solid with (g) be meter, institute
Europium nitrate (Eu (NO3) 3) is stated with (mol) as meter addition.
Preferably, 30min is sufficiently stirred under the revolving speed of the magnetic stirrer speed of agitator 500r/min.
Preferably, the centrifugation guarantees the of poor quality within ± 0.4g of every centrifuge tube, after being put into centrifuge, with
The speed of 600r/min is centrifuged 10min.
Preferably, solution is added no more than 70%-75% in the water heating kettle.
Preferably, the fluorophor performance test divides after taking out sample it is necessary to carry out crystal structure with X-ray diffractometer
Analysis, operating procedure is successively are as follows: one, with spoon take out bag in suitable powder, be added on glass slide drop-center, and use coverslip
Even spread；Two, after the tool after the test sample of powder is finished, spoon and coverslip require to use alcohol washes, dry；
Three, sample is put into detecting instrument, every group 10 minutes；Four, sample is carefully refunded to pack after the completion of detecting.
Compared with prior art, the beneficial effects of the present invention are:
1. the wiping by every sub-sampling product to tool is avoided and is impacted to subsequent operation, also avoids simultaneously
Error caused by inspection.
2. by having obtained good fluorescent powder proportion in the case of rigorous operating procedure and experiment high-dopant concentration while having adopted
Hydro-thermal method is a kind of efficient synthetic method, and the powder purity of preparation is high, and size of microcrystal is small and is evenly distributed, and is had required
The advantages that condition is uncomplicated, stable system.
In the present invention, it is not directed to part in the device and is the same as those in the prior art or can be realized by using the prior art,
Wiping of the present invention by every sub-sampling product to tool is avoided and is impacted to subsequent operation, while also avoiding examining
Caused by error；By having obtained good fluorescent powder proportion in the case of rigorous operating procedure and experiment high-dopant concentration while having adopted
Hydro-thermal method is a kind of efficient synthetic method, and the powder purity of preparation is high, and size of microcrystal is small and is evenly distributed, and is had required
The advantages that condition is uncomplicated, stable system.
Detailed description of the invention
Fig. 1 is each group powder sample result figure of the present invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
A kind of high-dopant concentration red fluorescence powder and preparation method thereof, comprising the following steps:
S1, the raw material for choosing manufacture high-dopant concentration red fluorescence powder include: wolframic acid ammonia (H40N10O41W12
XH2O), lanthanum nitrate (La (NO3) 3nH2O) and europium nitrate (Eu (NO3) 3) are raw material, and deionized water, ammonium hydroxide are solvent；
S2, select tool include: electronic balance, key, beaker, glass bar, pipette, 150ml volumetric flask, water heating kettle,
Centrifuge tube, centrifuge, magnetic stir bar, blender, baking oven, grinding rod, PH test paper and mortar；
S3, to raw material weigh: using electronic balance by upper table dosage requirements weighing La (NO3) 3 nH2O with
The solid of H40N10O41W12XH2O adds a small amount of deionized water to dissolve in small beaker respectively, and is sufficiently stirred, and is formed
Mixed liquor pipettes configured 3 solution of Eu (NO3) of specified amount with pipette again, then suitably adds deionized water, uses ammonium hydroxide
It adjusts solution and is 9 or so with PH test paper test solution PH；It is put into magnetic stir bar in the solution, is stirred with magnetic stirrer；
The solution being stirred and precipitating are packed into water heating kettle together, add appropriate amount of deionized water, and solution is divided into 4 by S4
4 groups of samples are moved into baking oven together, set constant 180 DEG C, time 12h of the position of drying temperature, carry out hydro-thermal reaction by group；
S5 takes out and completes the sample of hydro-thermal reaction and be centrifuged, removes supernatant liquor, then with appropriate amount of deionized water by powder
Move into centrifuge tube；
4 groups of centrifuge tubes are uniformly put into drying 48h or more in 80 DEG C of -85 DEG C of baking ovens, take out centrifuge tube, ground with mortar by S6
Be milled body 5-10min, envelope；
S7 takes out envelope finished product and carries out fluorophor performance test.
It is described weigh La (NO3) 3nH2O and H40N10O41W12XH2O solid with (g) be meter, the nitric acid
Europium (Eu (NO3) 3) is meter addition with (mol).
30min is sufficiently stirred under the revolving speed of the magnetic stirrer speed of agitator 500r/min.
The centrifugation guarantees the of poor quality within ± 0.4g of every centrifuge tube, after being put into centrifuge, with 600r/min's
Speed is centrifuged 10min.
Solution is added no more than 70%-75% in the water heating kettle.
After sample is taken out in the fluorophor performance test, crystal structure analysis will be carried out with X-ray diffractometer, be operated
Step is successively are as follows: one, with spoon take out bag in suitable powder, be added on glass slide drop-center, and uniformly applied with coverslip
Cloth；Two, after the tool after the test sample of powder is finished, spoon and coverslip require to use alcohol washes, dry；Three, sample
Product are put into detecting instrument, every group 10 minutes；Four, sample is carefully refunded to pack after the completion of detecting.
Specific embodiment scheme:
One, raw material materials record such as table 1；
Step 1: weigh: using electronic balance by upper table dosage requirement weighing group La (NO3) 3 nH2O with
The solid of H40N10O41W12XH2O.Step 2: dissolution: add a small amount of deionized water to dissolve in small beaker respectively, dissolve
It is drained and is mixed with glass bar afterwards, then pipette configured 3 solution of Eu (NO3) of specified amount with pipette, then suitably added and go
Ionized water, adjusting solution PH with ammonium hydroxide is 9 or so, continues to stir evenly to 35ml or so.
Step 3: stirring: being put into magnetic stir bar in the solution, stirs half an hour with magnetic stirrer, to reach dispersion
The effect of particle.
Step 4: it moves into baking oven: the solution being stirred and precipitating being packed into water heating kettle together, adds appropriate amount of deionized water, is
The safety of experiment pays attention to no more than 70%~80%, is otherwise easy during heating to cause because of gas expansion quick-fried
It is fried；5 groups of samples are moved into baking oven together, set constant 180 degrees Celsius of the position of drying temperature, the time is 12 hours, and it is anti-to carry out hydro-thermal
It answers.
Step 5: centrifugation: taking out the sample for completing hydro-thermal reaction, remove supernatant liquor, then with appropriate amount of deionized water by powder
End moves into centrifuge tube, guarantees the of poor quality within ± 0.5g of every centrifuge tube, protection centrifugation function normal use；It is put into centrifugation
After machine, 5min is centrifuged with the speed of 600r/min.
Step 6: 4 groups of centrifuge tubes uniformly drying: are put into drying 48h or more in 80 degrees Celsius of baking ovens.
Step 7: grinding envelope: centrifuge tube is taken out, with mortar grinder 5~10min of powder, envelope.
Table 1
Two, sample characterization and analysis:
Sample is carried out to the test of XRD and PL respectively.X-ray diffraction is made after 9 powder sample of La 2W 2O, will
Crystal structure analysis is carried out with X-ray diffractometer, specific steps are as follows.
Step 1: suitable powder in bag 1 is taken out with spoon, is added on glass slide drop-center, and uniform with coverslip
Coating.
Step 2: according to step 1, the test sample of 5 groups of powder after making is repeated；Pay attention to every group finish after, spoon and
Coverslip requires to use alcohol washes, dries.
Step 3: successively will test sample and be put into detecting instrument, every group 10 minutes.Step 4: by sample after the completion of detection
Carefully refund pack.Detecting step is completed, obtains each group powder sample result as shown in Figure 1:
In the present invention, wiping when use by every sub-sampling product to tool is avoided and is impacted to subsequent operation,
Error caused by examining is also avoided simultaneously；It is good by having been obtained in the case of rigorous operating procedure and experiment high-dopant concentration
The hydro-thermal method that fluorescent powder proportion uses simultaneously is a kind of efficient synthetic method, the powder purity height of preparation, size of microcrystal it is small and
It is evenly distributed, has many advantages, such as that required condition is uncomplicated, stable system.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (6)
1. a kind of high-dopant concentration red fluorescence powder and preparation method thereof, which comprises the following steps:
S1, the raw material for choosing manufacture high-dopant concentration red fluorescence powder include: wolframic acid ammonia (H40N10O41W12XH2O), nitre
Sour lanthanum (La (NO3) 3nH2O) and europium nitrate (Eu (NO3) 3) are raw material, and deionized water, ammonium hydroxide are solvent；
S2, select tool include: electronic balance, key, beaker, glass bar, pipette, 150ml volumetric flask, water heating kettle, centrifugation
Pipe, centrifuge, magnetic stir bar, blender, baking oven, grinding rod, PH test paper and mortar；
S3, to raw material weigh: using electronic balance by upper table dosage requirements weighing La (NO3) 3nH2O with
The solid of H40N10O41W12XH2O adds a small amount of deionized water to dissolve in small beaker respectively, and is sufficiently stirred, and is formed
Mixed liquor pipettes configured 3 solution of Eu (NO3) of specified amount with pipette again, then suitably adds deionized water, uses ammonium hydroxide
It adjusts solution and is 9 or so with PH test paper test solution PH；It is put into magnetic stir bar in the solution, is stirred with magnetic stirrer；
The solution being stirred and precipitating are packed into water heating kettle together, add appropriate amount of deionized water, and solution is divided into 4 groups, by 4 by S4
Group sample moves into baking oven together, sets constant 180 DEG C, time 12h of the position of drying temperature, carries out hydro-thermal reaction；
S5, the sample for taking out completion hydro-thermal reaction are centrifuged, and remove supernatant liquor, then moved into powder with appropriate amount of deionized water
Centrifuge tube；
4 groups of centrifuge tubes are uniformly put into drying 48h or more in 80 DEG C of -85 DEG C of baking ovens, centrifuge tube are taken out, with mortar grinder powder by S6
Body 5-10min, envelope；
S7 takes out envelope finished product and carries out fluorophor performance test.
2. a kind of high-dopant concentration red fluorescence powder according to claim 1 and preparation method thereof, which is characterized in that described
Weigh La (NO3) 3nH2O and H40N10O41W12XH2O solid with (g) be meter, the europium nitrate (Eu (NO3) 3)
It is meter addition with (mol).
3. a kind of high-dopant concentration red fluorescence powder according to claim 1 and preparation method thereof, which is characterized in that described
30min is sufficiently stirred under the revolving speed of magnetic stirrer speed of agitator 500r/min.
4. a kind of high-dopant concentration red fluorescence powder according to claim 1 and preparation method thereof, which is characterized in that described
Centrifugation guarantees the of poor quality within ± 0.4g of every centrifuge tube, after being put into centrifuge, is centrifuged with the speed of 600r/min
10min。
5. a kind of high-dopant concentration red fluorescence powder according to claim 1 and preparation method thereof, which is characterized in that described
Solution is added no more than 70%-75% in water heating kettle.
6. a kind of high-dopant concentration red fluorescence powder according to claim 1 and preparation method thereof, which is characterized in that described
After sample is taken out in fluorophor performance test, crystal structure analysis will be carried out with X-ray diffractometer, operating procedure is successively are as follows:
One, suitable powder in bag is taken out with spoon, be added on glass slide drop-center, and with coverslip even spread；Two, powder
After tool after test sample is finished, spoon and coverslip require to use alcohol washes, dry；Three, sample is put into detector
Device, every group 10 minutes；Four, sample is carefully refunded to pack after the completion of detecting.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006072447A1 (en) * | 2004-12-29 | 2006-07-13 | Hte Aktiengesellschaft | Phosphor-treated multimetallic oxide compounds |
| CN101418217A (en) * | 2008-10-29 | 2009-04-29 | 华南理工大学 | Multiple colour infrared up-conversion luminous material and preparing process thereof |
| CN101812296A (en) * | 2010-05-26 | 2010-08-25 | 哈尔滨师范大学 | Near ultraviolet or blue light excited tungstate red fluorescent powder and preparation method thereof |
-
2018
- 2018-06-21 CN CN201810641884.7A patent/CN109135743A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006072447A1 (en) * | 2004-12-29 | 2006-07-13 | Hte Aktiengesellschaft | Phosphor-treated multimetallic oxide compounds |
| CN101418217A (en) * | 2008-10-29 | 2009-04-29 | 华南理工大学 | Multiple colour infrared up-conversion luminous material and preparing process thereof |
| CN101812296A (en) * | 2010-05-26 | 2010-08-25 | 哈尔滨师范大学 | Near ultraviolet or blue light excited tungstate red fluorescent powder and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| XIAOFEI SHI ET AL.,: "Selective Crystallization of Four Tungstates (La2W3O12, La2W2O9, La14W8O45, and La6W2O15) via Hydrothermal Reaction and Comparative Study of Eu3+ Luminescence", 《INORG. CHEM.》 * |
| 丁柏林: "稀土元素Eu3+掺杂的La2W2O9粉体的制备与荧光性能表征", 《HTTPS://WENKU.BAIDU.COM/VIEW/800CE5C469DC5022ABEA006F.HTML》 * |
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Application publication date: 20190104 |