CN108998023A - A kind of phosphor host and preparation method thereof - Google Patents
A kind of phosphor host and preparation method thereof Download PDFInfo
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- CN108998023A CN108998023A CN201810770074.1A CN201810770074A CN108998023A CN 108998023 A CN108998023 A CN 108998023A CN 201810770074 A CN201810770074 A CN 201810770074A CN 108998023 A CN108998023 A CN 108998023A
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Abstract
The invention discloses a kind of phosphor hosts and preparation method thereof, first, in accordance with LiGd (MoO4)2The stoichiometric ratio of middle Gd and Mo element weighs Gd (NO respectively3)3·6H2O and Li2MoO4And be ground into powder and be dissolved in deionized water, respectively obtain solution A and solution B；Solution A is instilled in solution B, is stirred at room temperature to obtain mixing milky white solution；Milky white solution is mixed to neutral or alkalinity, and mineralizer is added and obtains precursor liquid；Precursor liquid is reacted at 240 DEG C again and generates white depositions for 24 hours, is cooled to room temperature；Then white depositions are separated and obtain intermediate product after being washed, be centrifuged and being dried；Finally intermediate product is calcined, obtains phosphor host；Select Gd (NO3)3·6H2O and Li2MoO4As raw material, element is essentially identical with object, will not introduce foreign ion and other phases in reaction process, and hydro-thermal method has that product good dispersion, reaction temperature is low, crystalline form is easy to control, the object of generation mutually purity is high；Hydro-thermal method preparation LiGd (MoO is filled up4)2For the blank of the luminescent material of matrix.
Description
Technical field
The invention belongs to rare earth luminescent material fields, and in particular to a kind of phosphor host and preparation method thereof.
Background technique
Most of fluorescent powder is made of matrix and activator.Matrix is the host compound of luminescent material, is by having
The crystal for having certain crystallographic structure stable serves as.There are many kinds of the materials that can be used as fluorescent powder matrix, wherein having scheelite knot
Double molybdates of structure receive the extensive concern of people, such compound has stable physics and chemical property.
In the large family of double molybdates, LiGd (MoO4)2Belong to tetragonal phase, has been used for the host material of fluorescent powder.Mesh
Preceding preparation LiGd (MoO4)2Method be mainly high temperature solid-state method.Compared with high temperature solid-state method, hydro-thermal method has product dispersibility
Well, the advantages that reaction temperature is low, crystalline form is easy to control.But since Li ionic radius is too small, the reason of hardly entering bonding in lattice,
So far LiGd (MoO is successfully prepared without discovery hydro-thermal method4)2Report.Therefore phosphor host LiGd (MoO4)2Using
The successful preparation of hydro-thermal method, the influence research of pattern and structure to luminescent properties to fluorescent powder have great importance.
Summary of the invention
In order to solve problems of the prior art, the invention discloses a kind of phosphor host and its preparations
Method, phosphor host are LiGd (MoO4)2, a blank in preparation method field has been filled up, for LiGd
(MoO4)2It lays a good foundation for the luminescent material pattern of matrix and the research of structure.
To achieve the goals above, the technical solution adopted by the present invention is that, a kind of preparation method of phosphor host,
The following steps are included:
Step 1, according to LiGd (MoO4)2The stoichiometric ratio of middle Gd and Mo element weighs Gd (NO respectively3)3·6H2O and
Li2MoO4And be ground into powder and be dissolved in deionized water, respectively obtain solution A and solution B；
Step 2, step 1 acquired solution A is instilled in solution B, is stirred at room temperature to obtain mixing milky white solution；
Step 3, mixing milky white solution obtained by regulating step 2 is to neutral or alkalinity, and mineralizer is added and obtains precursor liquid；
Step 4, precursor liquid obtained by step is reacted at 240 DEG C and generates white depositions for 24 hours, be cooled to room temperature；
Step 5,4 gained white depositions of separating step by washing and be centrifuged, then obtain intermediate production after being dried
Object；
Step 6, by 600 DEG C in air atmosphere~640 DEG C calcining 3h~5h of step 5 gained intermediate product, fluorescence is obtained
Powder host material.
In step 2, solution A is slowly dropped into solution B.
In step 2, using magnetic agitation, mixing time is 60min~80min.
The pH of mixed solution is adjusted using LiOH solution in step 3, and the range of pH value is 7~10.
Added mineralizer is urea in step 3, and addition urea makes its concentration 0.15mol/L~0.35mol/L.
Step 4 gained precursor liquid seals reaction, the filling of reaction kettle volume in the stainless steel cauldron of polyparaphenylene liner
Degree is 65%.
Step 5 gained white depositions are by water and ethyl alcohol alternately washing 3 times；Centrifugal rotational speed is 10000r/min, centrifugation
Time 3min；The dry 10h at 75 DEG C of temperature.
Using step 1~5 the methods preparation phosphor host.
Compared with prior art, the present invention, which at least has the advantages that, selects Gd (NO3)3·6H2O and Li2MoO4Make
For raw material, element is identical as object, and foreign ion will not be introduced in reaction process and generates other phases, is conducive to improve production
Object purity, and hydro-thermal reaction at relatively high temperatures, facilitate object and mutually crystallize；Li2MoO4Two members needed for object is provided
Element greatly simplifies preparation process；In addition, hydro-thermal method has, product good dispersion, reaction temperature is low, crystalline form is easy to control, raw
At object mutually purity is high；The present invention has filled up hydrothermal synthesis method and has prepared fluorescent powder LiGd (MoO4)2Blank, for LiGd
(MoO4)2It lays a good foundation for the luminescent material pattern of matrix and the research of structure.
Further, the impurity element that not will increase final product as mineralizer using urea is conducive to improve product
Purity.
Further, using polyparaphenylene as inner liner of reaction kettle, it is ensured that 240 DEG C of hydro-thermal reactions are gone on smoothly.
Detailed description of the invention
Fig. 1 is the XRD spectrum of intermediate product powder after the completion of hydro-thermal reaction in embodiment 3.
Fig. 2 is the TG-DSC map of intermediate product powder after the completion of hydro-thermal reaction in embodiment 3.
Fig. 3 is powder LiGd (MoO after the completion of the calcining of 3 intermediate product of embodiment4)2XRD spectrum.
Fig. 4 is powder LiGd (MoO after the completion of hydro-thermal reaction in embodiment 34)2SEM figure.
Fig. 5 is powder LiGd (MoO after calcining after the completion of hydro-thermal reaction in embodiment 34)2SEM figure.
Specific embodiment
The present invention is described in further details below in conjunction with attached drawing and specific embodiment.
A kind of phosphor host LiGd (MoO4)2And preparation method thereof,
Embodiment 1:
LiGd (MoO is prepared by following steps4)2:
(1) according to LiGd (MoO4)2The stoichiometric ratio of middle Gd and Mo element weighs the Gd (NO of 3.5mmol respectively3)3·
6H2The Li of O and 7mmol2MoO4And be ground into powder and be dissolved in deionized water, respectively obtain solution A and solution B；
(2) solution A in step (1) is slowly dropped into solution B, magnetic agitation 60min obtains mixing milky white at room temperature
Solution；
(3) it selects the pH of mixing milky white solution in LiOH solution regulating step (2) to be 7 and urea is added, makes the dense of urea
Degree is 0.15mol/L, obtains precursor liquid；
(4) precursor liquid obtained by step (3) is moved into the stainless steel cauldron of polyparaphenylene liner, the filling of reaction kettle volume
Degree is 65%, generates white depositions for 24 hours in 240 DEG C of sealing reactions, is cooled to room temperature；
(5) white depositions obtained by separating step (4) are centrifuged after water and ethyl alcohol alternately wash 3 times, are then placed in 75
Intermediate product is obtained after dry 10h in DEG C drying box；
(6) by intermediate product obtained by step (5), 600 DEG C of calcining 3h obtain pure phase substance LiGd in air atmosphere
(MoO4)2。
Embodiment 2:
LiGd (MoO is prepared by following steps4)2:
(1) according to LiGd (MoO4)2The stoichiometric ratio of middle Gd and Mo element weighs the Gd (NO of 3.5mmol respectively3)3·
6H2The Li of O and 7mmol2MoO4And be ground into powder and be dissolved in deionized water, respectively obtain solution A and solution B；
(2) step (1) acquired solution A is slowly dropped into solution B, then magnetic agitation 70min is mixed at room temperature
Milky white solution；
(3) selecting the pH of mixing milky white solution obtained by LiOH solution regulating step (2) is 8, and urea is added, and makes urea
Concentration is 0.25mol/L, obtains precursor liquid；
(4) precursor liquid obtained by step (3) is moved into the stainless steel cauldron of polyparaphenylene liner, the filling of reaction kettle volume
Degree is 65%, generates white depositions for 24 hours in 240 DEG C of sealing reactions, is cooled to room temperature；
(5) white depositions obtained by separating step (4) are centrifuged after water and ethyl alcohol alternately wash 3 times, are then put
Enter in 75 DEG C of drying boxes and obtains intermediate product after dry 10h；
(6) by intermediate product obtained by step (5), 625 DEG C of calcining 4h obtain pure phase substance LiGd in air atmosphere
(MoO4)2。
Embodiment 3:
LiGd (MoO is prepared by following steps4)2:
(1) according to LiGd (MoO4)2The stoichiometric ratio of middle Gd and Mo element weighs the Gd (NO of 3.5mmol respectively3)3·
6H2The Li of O and 7mmol2MoO4And be ground into powder and be dissolved in deionized water, respectively obtain solution A and solution B；
(2) by step (1) acquired solution A be slowly dropped into solution B at room temperature magnetic agitation 80min obtain mixing it is milky white molten
Liquid；
(3) pH=9 of mixing milky white solution obtained by LiOH solution regulating step (2) is selected, and urea is added, makes urea
Concentration is 0.25mol/L, obtains precursor liquid；
(4) precursor liquid obtained by step (3) is moved into the stainless steel cauldron of polyparaphenylene liner, the filling of reaction kettle volume
Degree is 65%, generates white depositions for 24 hours in 240 DEG C of sealing reactions, is cooled to room temperature；
(5) white depositions obtained by separating step (4) are centrifuged after water and ethyl alcohol alternately wash 3 times, are placed into
Intermediate product is obtained after dry 10h in 75 DEG C of drying boxes；
(6) by intermediate product obtained by step (5), 625 DEG C of calcining 5h obtain pure phase substance LiGd in air atmosphere
(MoO4)2。
Fig. 1 is the XRD spectrum of intermediate product powder after the completion of the present embodiment hydro-thermal reaction, it can be determined that working as from figure
Preceding object is mutually reactant by obtained middle transition product under high-temperature and high-pressure conditions, is carried out to the middle transition product
Target product LiGd (MoO can be obtained in calcination processing4)2。
Fig. 2 is the TG-DSC map of intermediate product powder after the completion of hydro-thermal reaction in the present embodiment, as can be seen from the figure
In 600~640 DEG C of temperature ranges, sample has an apparent endothermic peak and the reduction along with quality, it is seen that warm herein
The crystallization process of phase transition has occurred in sample in degree range, and has carried out XRD test to this sample.
Fig. 3 is the present embodiment intermediate product powder LiGd (MoO after 625 DEG C of calcining 5h4)2XRD spectrum, it is bright from figure
It is aobvious to find out, the XRD test result and LiGd (MoO of sample4)2PDF card meet and preferably show prepared sample by forging
The recrystallization process that phase transition has occurred after burning processing, ultimately forms the LiGd (MoO of pure phase4)2。
Fig. 4 is powder LiGd (MoO after the completion of the present embodiment hydro-thermal reaction4)2SEM spectrum, Fig. 5 be the present embodiment calcining
Powder LiGd (MoO after the completion4)2SEM spectrum, the pattern of sample is the smooth nanometer sheet in surface, calcination processing before calcination processing
It is afterwards the nanometer sheet shaped like oatmeal.
Embodiment 4:
LiGd (MoO is prepared by following steps4)2:
(1) according to LiGd (MoO4)2The stoichiometric ratio of middle Gd and Mo element weighs the Gd (NO of 3.5mmol respectively3)3·
6H2The Li of O and 7mmol2MoO4And be ground into powder and be dissolved in deionized water, respectively obtain solution A and solution B；
(2) step (1) acquired solution A is slowly dropped into solution B, magnetic agitation 80min obtains mixing milky white at room temperature
Solution；
(3) pH=10 of mixing milky white solution obtained by LiOH solution regulating step (2) is selected, and urea is added, makes urea
Concentration be 0.35mol/L, obtain precursor liquid；
(4) precursor liquid obtained by step (3) is moved into the stainless steel cauldron of polyparaphenylene liner, the filling of reaction kettle volume
Degree is 65%, generates white depositions for 24 hours in 240 DEG C of sealing reactions, is cooled to room temperature；
(5) white depositions obtained by separating step (4) are alternately washed 3 times and are centrifuged by water and ethyl alcohol, place into
Intermediate product is obtained after dry 10h in 75 DEG C of drying boxes；
(6) by intermediate product obtained by step (5), 640 DEG C of calcining 5h obtain pure phase substance LiGd in air atmosphere
(MoO4)2。
The foregoing is merely better embodiments of the invention, are not unique embodiments, all in spirit of the invention
Within principle, any modification made under without departing from this technical process, equivalent replacement, improve etc., it is power of the invention
Benefit requires to be covered.
Claims (8)
1. a kind of preparation method of phosphor host, which comprises the following steps:
Step 1, according to LiGd (MoO4)2The stoichiometric ratio of middle Gd and Mo element weighs Gd (NO respectively3)3·6H2O and Li2MoO4
And be ground into powder and be dissolved in deionized water, respectively obtain solution A and solution B；
Step 2, step 1 acquired solution A is instilled in solution B, is stirred at room temperature to obtain mixing milky white solution；
Step 3, mixing milky white solution obtained by regulating step 2 is to neutral or alkalinity, and mineralizer is added and obtains precursor liquid；
Step 4, precursor liquid obtained by step is reacted at 240 DEG C and generates white depositions for 24 hours, be cooled to room temperature；
Step 5,4 gained white depositions of separating step obtain intermediate product by washing and being centrifuged, then after being dried；
Step 6, by 600 DEG C in air atmosphere~640 DEG C calcining 3h~5h of step 5 gained intermediate product, fluorescent powder base is obtained
Material.
2. a kind of preparation method of phosphor host according to claim 1, which is characterized in that in step 2, solution
A is slowly dropped into solution B.
3. a kind of preparation method of phosphor host according to claim 1, which is characterized in that in step 2, use
Magnetic agitation, mixing time are 60min~80min.
4. a kind of preparation method of phosphor host according to claim 1, which is characterized in that mixed in step 3
The pH of solution is adjusted using LiOH solution, and the range of pH value is 7~10.
5. a kind of preparation method of phosphor host according to claim 1, which is characterized in that added in step 3
The mineralizer added is urea, and addition urea makes its concentration 0.15mol/L~0.35mol/L.
6. a kind of preparation method of phosphor host according to claim 1, which is characterized in that before obtained by step 4
It drives liquid and seals reaction in the stainless steel cauldron of polyparaphenylene liner, reaction kettle volume compactedness is 65%.
7. a kind of preparation method of phosphor host according to claim 1, which is characterized in that white obtained by step 5
Color sediment is by water and ethyl alcohol alternately washing 3 times；Centrifugal rotational speed is 10000r/min, centrifugation time 3min；At 75 DEG C of temperature
Lower dry 10h.
8. a kind of phosphor host prepared using any one of claim 1~6 the method.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109911937A (en) * | 2019-02-01 | 2019-06-21 | 渤海大学 | A kind of NaRE (MoO4)2From sacrifice method for preparing template |
| CN110551500A (en) * | 2019-09-05 | 2019-12-10 | 陕西科技大学 | DTAB-assisted red fluorescent powder with enhanced luminescence property and preparation method thereof |
| CN112980439A (en) * | 2021-02-26 | 2021-06-18 | 陕西科技大学 | Molybdate-based fluorescent powder and preparation method thereof |
-
2018
- 2018-07-13 CN CN201810770074.1A patent/CN108998023B/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109911937A (en) * | 2019-02-01 | 2019-06-21 | 渤海大学 | A kind of NaRE (MoO4)2From sacrifice method for preparing template |
| CN109911937B (en) * | 2019-02-01 | 2021-01-22 | 渤海大学 | NaRE (MoO)4)2Preparation method of self-sacrifice template |
| CN110551500A (en) * | 2019-09-05 | 2019-12-10 | 陕西科技大学 | DTAB-assisted red fluorescent powder with enhanced luminescence property and preparation method thereof |
| CN110551500B (en) * | 2019-09-05 | 2021-03-23 | 陕西科技大学 | DTAB-assisted red fluorescent powder with enhanced luminescence property and preparation method thereof |
| CN112980439A (en) * | 2021-02-26 | 2021-06-18 | 陕西科技大学 | Molybdate-based fluorescent powder and preparation method thereof |
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