CN110272741A - A kind of germanate red fluorescence powder and preparation method thereof - Google Patents
A kind of germanate red fluorescence powder and preparation method thereof Download PDFInfo
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Abstract
The present invention discloses a kind of germanate red fluorescence powder, and the chemical general formula of germanate red fluorescence powder is M3La2‑x‑yGe3O12:(xEu3+ySm3+), it cannot be 0 that wherein M is one of Sr, Ca, 0≤x≤1.0,0≤y≤0.2, and x, y simultaneously.The present invention also provides a kind of preparation method of germanate red fluorescence powder, include the following steps: that (1) by than weighing reaction raw materials, is mixed in mixing tank；(2) fluxing agent is added in mixing tank, stirs evenly, fluxing agent H3BO3、NH4Cl and NH4One of F or more than one；(3) raw material of mixing is calcined, temperature is 1000~1500 DEG C, and calcination time is 2~20h, is subsequently cooled to 200 DEG C hereinafter, taking out, broken, grinding, pickling, deionized water is washed till neutrality, dries, and is sieved to get red fluorescence powder.Germanate red fluorescence powder of the invention, synthesis temperature is lower, easy to industrialized production in preparation process.The fluorescent powder being prepared with the method for the present invention absorbs by force in ultra-violet (UV) band, and stability is good, luminance is high, has excellent performance.
Description
Technical field
The present invention relates to field of light emitting materials more particularly to a kind of germanate red fluorescence powder and preparation method thereof.
Background technique
The advantages that white light LEDs have environmental protection as a kind of forth generation green light source, and energy conservation, efficiently, response are fast, and the service life is long,
It is studied by more and more researchers.Realize that the mode of white light LEDs has " (usually by the LED chip of different colours at present
Red-green-blue) collect the white light for merging and blending together " and " blue chip+YAG yellow fluorescent powder is mixed to get white light " two schemes,
But in the former combination, the bias of different chips is different, requires height to circuit control, causes at high cost, it is difficult to answer extensively
With；The latter's YAG fluorescent powder lacks the ingredient of feux rouges, and there are colour temperature is higher (being usually located at 5000K~7500K), colour rendering index
Relatively low (Ra is 70~75), while blue light has overflow problem, accumulates over a long period, human eye retina will will receive irreversible wound
Evil.To solve this problem, in recent years many researchers propose utilization " near ultraviolet chip (395~400nm)+red,
Green, blue three primary colors fluorescent powder obtains white light " scheme, this wave band ultraviolet light has high luminous intensity, while can pass through addition
Different fluorescent powders adjusts the optical characteristics of white light LED part, simple and easy.It is commercial near ultraviolet excitated on the market simultaneously
Y2O2S:Eu rouge and powder, stability is poor, and energy conversion efficiency is low, and sulfide rouge and powder easily corrodes chip set etc..In view of
This, needs that a kind of simple process, luminous intensity be high, has good stability, and the germanate red that can be widely applied to LED field is glimmering
Light powder.
Summary of the invention
For overcome the deficiencies in the prior art, the purpose of the present invention is to provide a kind of simple process, luminous intensity are high, steady
It is qualitative good, it can be widely applied to the germanate red fluorescence powder of LED field.
The purpose of the present invention is implemented with the following technical solutions:
A kind of germanate red fluorescence powder, the chemical general formula of germanate red fluorescence powder are M3La2-x-yGe3O12:(xEu3+
ySm3+), it cannot be 0 that wherein M is one of Sr, Ca, 0≤x≤1.0,0≤y≤0.2, and x, y simultaneously.
The present invention also provides a kind of preparation methods of germanate red fluorescence powder, include the following steps:
(1) reaction raw materials are weighed by the stoichiometric ratio of M, La, Ge, Eu and Sm ion in chemical formula, is mixed in mixing
In tank；
(2) fluxing agent is added in mixing tank, stirs evenly, fluxing agent H3BO3、NH4Cl and NH4One of F or one
Kind or more；
(3) raw material of mixing is calcined, temperature is 1000~1500 DEG C, and calcination time is 2~20h, is then cooled down
It to 200 DEG C hereinafter, taking out, is crushed, grinding, pickling, deionized water is washed till neutrality, dries, and is sieved to get red fluorescence powder.
In one of specific embodiment of the invention, in step (1) reaction raw materials, when M is Sr, corresponding reaction
Raw material is SrCO3, SrO and SrC2O4In any one；When M is Ca, corresponding reaction raw materials are CaCO3, CaO and CaC2O4In
Any one.
SrCO3、SrO、SrC2O4、CaCO3, CaO and CaC2O4Under calcination temperature of the present invention, it is decomposed to form corresponding oxidation
Object, the gas of generation are CO2, will not influence the performance of product and remove remaining reaction raw materials convenient for later period acid adding.
In one of specific embodiment of the invention, in step (1) reaction raw materials, the corresponding reaction raw materials of La are
La2O3、La2(CO3)3With La (NO3)3In any one.La2O3, La2(CO3)3With La (NO3)3Under calcination temperature of the present invention,
It is decomposed to form corresponding oxide and participates in reaction, remove remaining reaction raw materials convenient for later period acid adding.
In one of specific embodiment of the invention, in step (1) reaction raw materials, the corresponding reaction raw materials of Ge are
GeO2。
In one of specific embodiment of the invention, in step (1) reaction raw materials, the corresponding reaction raw materials of Eu are
Eu2O3With Eu (NO3)3·6H2Any one in O or two kinds；The corresponding reaction raw materials of Sm are Sm2O3With Sm (NO3)3·6H2O
In any one or two kinds.
In one of specific embodiment of the invention, the additive amount of step (2) fluxing agent is the reaction original weighed
Expect the 0.1%~3.0% of gross mass.When 0.1%~3.0% that the additive amount of fluxing agent is the reaction raw materials gross mass weighed
When, obtained germanate red fluorescence powder crystal form rule, luminous efficiency is high, and performance is stablized.
In one of specific embodiment of the invention, the pickling of step (3), using the HCl of pH=3.0~6.0
Solution.HCl solution by adding pH=3.0~6.0 can rapidly remove the reaction raw materials that reaction is not engaged in product, acid
Property too strong luminescent properties to product there is strong influence.
Compared with prior art, the beneficial effects of the present invention are:
Germanate red fluorescence powder of the invention provides a kind of new formula for the preparation of red fluorescence powder.Preparation process
Middle synthesis temperature is lower, simple for process, easy to industrialized production.The fluorescent powder being prepared with the method for the present invention is ultraviolet
Area absorbs by force, and stability is good, luminance is high, has excellent performance, and can be used near ultraviolet chip (395~400nm) encapsulation white light LEDs
Device.
Detailed description of the invention
Fig. 1 is the XRD spectrum that the present invention implements embodiment 1.
Fig. 2 is the excitation spectrum and emission spectrum that the present invention implements fluorescent powder made from embodiment 1.
Fig. 3 is the excitation spectrum and emission spectrum that the present invention implements fluorescent powder made from embodiment 2.
Fig. 4 is the excitation spectrum and emission spectrum that the present invention implements fluorescent powder made from embodiment 3.
Fig. 5 is the excitation spectrum and emission spectrum that the present invention implements fluorescent powder made from embodiment 4.
Fig. 6 is the excitation spectrum and emission spectrum that the present invention implements fluorescent powder made from embodiment 5.
Fig. 7 is the excitation spectrum and emission spectrum that the present invention implements fluorescent powder made from embodiment 6.
Fig. 8 is the excitation spectrum and emission spectrum that the present invention implements fluorescent powder made from embodiment 7.
Specific embodiment
The embodiments described below with reference to the accompanying drawings are exemplary, for explaining only the invention, and should not be understood as
Limitation of the present invention.
A kind of germanate red fluorescence powder, the chemical general formula of germanate red fluorescence powder are M3La2-x-yGe3O12:(xEu3+
ySm3+), it cannot be 0 that wherein M is one of Sr, Ca, 0≤x≤1.0,0≤y≤0.2, and x, y simultaneously.
The present invention also provides a kind of preparation methods of germanate red fluorescence powder, include the following steps:
(1) reaction raw materials are weighed by the stoichiometric ratio of M, La, Ge, Eu and Sm ion in chemical formula, is mixed in mixing
In tank；
(2) fluxing agent is added in mixing tank, stirs evenly, fluxing agent H3BO3、NH4Cl and NH4One of F or one
Kind or more；
(3) raw material of mixing is calcined, temperature is 1000~1500 DEG C, and calcination time is 2~20h, is then cooled down
It to 200 DEG C hereinafter, taking out, is crushed, grinding, pickling, deionized water is washed till neutrality, dries, and is sieved to get red fluorescence powder.
In one of specific embodiment of the invention, in step (1) reaction raw materials, when M is Sr, corresponding reaction
Raw material is SrCO3, SrO and SrC2O4In any one；When M is Ca, corresponding reaction raw materials are CaCO3, CaO and CaC2O4In
Any one.
SrCO3、SrO、SrC2O4、CaCO3, CaO and CaC2O4Under calcination temperature of the present invention, it is decomposed to form corresponding oxidation
Object, the gas of generation are CO2, will not product performance and remove remaining reaction raw materials convenient for later period acid adding.
In one of specific embodiment of the invention, in step (1) reaction raw materials, the corresponding reaction raw materials of La are
La2O3、La2(CO3)3With La (NO3)3In any one.La2O3, La2(CO3)3With La (NO3)3Under calcination temperature of the present invention,
It is decomposed to form corresponding oxide and participates in reaction, remove remaining reaction raw materials convenient for later period acid adding.
In one of specific embodiment of the invention, in step (1) reaction raw materials, the corresponding reaction raw materials of Ge are
GeO2。
In one of specific embodiment of the invention, in step (1) reaction raw materials, the corresponding reaction raw materials of Eu are
Eu2O3With Eu (NO3)3·6H2Any one in O or two kinds；The corresponding reaction raw materials of Sm are Sm2O3With Sm (NO3)3·6H2O
In any one or two kinds.
In one of specific embodiment of the invention, the additive amount of step (2) fluxing agent is the reaction original weighed
Expect the 0.1%~3.0% of gross mass.When 0.1%~3.0% that the additive amount of fluxing agent is the reaction raw materials gross mass weighed
When, obtained germanate red fluorescence powder crystal form rule, luminous efficiency is high, and performance is stablized.
In one of specific embodiment of the invention, the pickling of step (3), using the HCl of pH=3.0~6.0
Solution.HCl solution by adding pH=3.0~6.0 can rapidly remove, and the reaction raw materials of reaction are not engaged in product.
Embodiment 1
Sr3La1.97Ge3O12:0.03Sm3+The preparation method of fluorescent powder, includes the following steps:
8.18g SrCO is accurately weighed in proportion3、5.93g La2O3、5.80g GeO2、0.097g Sm2O3And 0.09g
H3BO3It is added in mixing tank, being sufficiently stirred makes its mixing.The raw material of mixing is transferred in 20mL corundum crucible.Crucible is put into
In Muffle furnace, calcining 8h is carried out in 1200 DEG C.Sample grinding is taken out after temperature in burner hearth is down to 200 DEG C or less, and uses pH=
3.0 HCl solution carries out pickling, and deionized water is washed till neutrality.It finally dries sample, is sieved to obtain the final product.It is found, is obtained by test
The fluorescent powder of pure phase structure, XRD are as shown in Figure 1.The excitation and emission spectra of fluorescent powder as shown in Fig. 2, as seen from the figure its
It is suitable near ultraviolet chip (395~400nm) excitation.
Embodiment 2
Sr3La1.94Ge3O12:0.06Eu3+The preparation method of fluorescent powder, includes the following steps:
5.67g SrO, 8.10g La are accurately weighed in proportion2(CO3)3、5.73g GeO2、0.49g Eu(NO3)3·
6H2O、0.09g H3BO3With 0.06g NH4Cl is added in mixing tank, and being sufficiently stirred makes its mixing.The raw material of mixing is placed in
In 20mL corundum crucible and be transferred in Muffle furnace, carry out calcining 2h in 1500 DEG C, to temperature in burner hearth be down to 200 DEG C hereinafter,
It takes out sample grinding, and carries out pickling with the HCl solution of pH=5.0, deionized water is washed till neutrality, and drying is sieved to obtain the final product.Its is glimmering
The excitation and emission spectra of light powder is as shown in Figure 3.
Embodiment 3
Sr3La1.0Ge3O12:1.0Eu3+The preparation method of fluorescent powder, includes the following steps:
7.27g SrC is accurately weighed in proportion2O4、5.97g La(NO3)3·6H2O、4.33g GeO2、7.26g Eu2O3、
0.35gNH4Cl and 0.25g NH4F is added in mixing tank, and being sufficiently stirred makes its mixing.The raw material of mixing is placed in corundum crucible
In, it is put into Muffle furnace, carries out calcining 20h in 1000 DEG C, be down to 200 DEG C to temperature in burner hearth and ground hereinafter, taking out sample
Mill, and pickling is carried out with the HCl solution of pH=3.5, deionized water is washed till neutrality, and drying is sieved to obtain the final product.The excitation of its fluorescent powder
It is as shown in Figure 4 with emission spectrum.
Embodiment 4
Sr3La1.67Ge3O12:(0.3Eu3+,0.03Sm3+) fluorescent powder preparation method, include the following steps:
8.36g SrCO is accurately weighed in proportion3、5.74g La2O3、4.98g GeO2、0.84g Eu2O3、0.083g
Sm2O3With 0.13g H3BO3It is added in mixing tank, being sufficiently stirred makes its mixing.The raw material of mixing is placed in corundum crucible, is put
Enter in Muffle furnace, carry out calcining 4h in 1400 DEG C, is down to 200 DEG C to temperature in burner hearth and is crushed, ground hereinafter, taking out sample
Mill, and pickling is carried out with the HCl solution of pH=3.0, deionized water is washed till neutrality, and drying is sieved to obtain the final product.The excitation of its fluorescent powder
It is as shown in Figure 5 with emission spectrum.
Embodiment 5
Ca3La1.99Ge3O12:0.01Sm3+The preparation method of fluorescent powder, includes the following steps:
5.72g CaCO is accurately weighed in proportion3、8.21g La2O3、5.98g GeO2、0.082g Sm(NO3)3·6H2O
With 0.15g H3BO3It is added in mixing tank, being sufficiently stirred makes its mixing.The raw material of mixing is placed in corundum crucible, Muffle is put into
In furnace, calcining 2.5h is carried out in 1450 DEG C, 200 DEG C is down to temperature in burner hearth and is ground hereinafter, taking out sample, and use pH=
4.0 HCl solution carries out pickling, and deionized water is washed till neutrality, dries, is sieved to obtain the final product.The excitation and emission spectra of its fluorescent powder
As shown in Figure 6.
Embodiment 6
Ca3La1.4Ge3O12:0.6Eu3+The preparation method of fluorescent powder, includes the following steps:
3.19g CaO, 5.76g La are accurately weighed in proportion2(CO3)3、5.96g GeO2、5.08g Eu(NO3)3·6H2O
With 0.42g NH4F is added in mixing tank, and being sufficiently stirred makes its mixing.The raw material of mixing is placed in corundum crucible, Muffle is put into
In furnace, calcining 6h is carried out in 1300 DEG C, 200 DEG C is down to temperature in burner hearth and is ground hereinafter, taking out sample, and use pH=
6.0 HCl solution carries out pickling, and deionized water is washed till neutrality, dries, is sieved to obtain the final product.The excitation and emission spectra of its fluorescent powder
As shown in Figure 7.
Embodiment 7
Ca3La1.48Ge3O12:(0.5Eu3+,0.02Sm3+) fluorescent powder preparation method, include the following steps:
4.89g CaC is accurately weighed in proportion2O4、8.16g La(NO3)3、3.99g GeO2、2.84g Eu(NO3)3·
6H2O、0.11g Sm(NO3)3·6H2O、0.10g H3BO3With 0.33g NH4Cl is added in mixing tank, and being sufficiently stirred keeps it mixed
It is even.The raw material of mixing is placed in corundum crucible, is put into Muffle furnace, carries out calcining 15h in 1150 DEG C, is dropped to temperature in burner hearth
It is ground to 200 DEG C hereinafter, taking out sample, and carries out pickling with the HCl solution of pH=4.5, deionized water is washed till neutrality, dries
It is dry, it is sieved to obtain the final product.The excitation and emission spectra of its fluorescent powder is as shown in Figure 8.
Above embodiment is only certain preferred embodiments of the invention, cannot limit the model protected of the present invention with this
It encloses, the variation and replacement for any unsubstantiality that those skilled in the art is done on the basis of the present invention belong to the present invention
Range claimed.
Claims (8)
1. a kind of germanate red fluorescence powder, which is characterized in that the chemical general formula of the germanate red fluorescence powder is M3La2-x- yGe3O12:(xEu3+ySm3+), it cannot be 0 that wherein M is one of Sr, Ca, 0≤x≤1.0,0≤y≤0.2, and x, y simultaneously.
2. a kind of preparation method of germanate red fluorescence powder as described in claim 1, which comprises the steps of:
(1) reaction raw materials are weighed by the stoichiometric ratio of M, La, Ge, Eu and Sm ion in chemical formula, is mixed in mixing tank；
(2) fluxing agent is added in mixing tank, stirs evenly, fluxing agent H3BO3、NH4Cl and NH4One of F or a kind of with
On；
(3) raw material of mixing is calcined, temperature is 1000~1500 DEG C, and calcination time is 2~20h, is subsequently cooled to 200
DEG C hereinafter, take out, it is crushed, grinding, pickling, deionized water is washed till neutrality, dries, and is sieved to get red fluorescence powder.
3. the preparation method of red fluorescence powder according to claim 2, which is characterized in that step (1) described reaction raw materials
In, when M is Sr, the corresponding reaction raw materials are SrCO3, SrO and SrC2O4In any one；When M is Ca, corresponding institute
Stating reaction raw materials is CaCO3, CaO and CaC2O4In any one.
4. the preparation method of red fluorescence powder according to claim 2, which is characterized in that step (1) described reaction raw materials
In, the corresponding reaction raw materials of La are La2O3、La2(CO3)3With La (NO3)3In any one.
5. the preparation method of red fluorescence powder according to claim 2, which is characterized in that step (1) described reaction raw materials
In, the corresponding reaction raw materials of Ge are GeO2。
6. the preparation method of red fluorescence powder according to claim 2, which is characterized in that step (1) described reaction raw materials
In, the corresponding reaction raw materials of Eu are Eu2O3With Eu (NO3)3·6H2Any one in O or two kinds；Sm is corresponding described anti-
Answering raw material is Sm2O3With Sm (NO3)3·6H2Any one in O or two kinds.
7. the preparation method of red fluorescence powder according to claim 2, which is characterized in that step (2) described fluxing agent
Additive amount is the 0.1%~3.0% of the reaction raw materials gross mass weighed.
8. the preparation method of red fluorescence powder according to claim 2, which is characterized in that pickling described in step (3) is adopted
With the HCl solution of pH=3.0~6.0.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112625683A (en) * | 2020-12-30 | 2021-04-09 | 中国地质大学（北京） | Germanate type red fluorescent powder and preparation method thereof |
| CN116814260A (en) * | 2023-06-19 | 2023-09-29 | 昆明学院 | Magnesium calcium germanate fluorescent powder and preparation method thereof |
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| CN105271760A (en) * | 2015-11-05 | 2016-01-27 | 中国科学院福建物质结构研究所 | Glass ceramics for AC-LED and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116814260A (en) * | 2023-06-19 | 2023-09-29 | 昆明学院 | Magnesium calcium germanate fluorescent powder and preparation method thereof |
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Application publication date: 20190924 |