CN105860973B - A kind of magnesium Indium phosphate red or green emitting phosphor and its preparation - Google Patents
A kind of magnesium Indium phosphate red or green emitting phosphor and its preparation Download PDFInfo
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- C09K11/70—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing phosphorus
- C09K11/71—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing phosphorus also containing alkaline earth metals
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- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
- C09K11/7737—Phosphates
- C09K11/7738—Phosphates with alkaline earth metals
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- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7743—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing terbium
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Abstract
A kind of magnesium Indium phosphate is red or green emitting phosphor and its preparation, its chemical formula are Mg21‑28(In1‑xLnx)28‑34P42‑48Oy(x=0.02~0.11, y=168~199), wherein Ln are rare earth ion Eu or Tb.In the fluorescent material, with novel phosphoric acid salt compound Mg21‑28In28‑34P42‑48Oy(y=168 199) is matrix, by adulterating different rare earth elements in the matrix, can be obtained under burst of ultraviolel, has the fluorescent material of intense emission in different spectral regions.The preparation method uses wet-chemical solid sintering technology.The fluorescent material of the present invention has good optical property, and can meet the requirement of three-color fluorescent lamp very well.
Description
Technical field：
It is red more particularly, to the one kind that can apply to three-color fluorescent lamp the present invention relates to rare earth luminescent material field
Or green rare-earth phosphate base fluorescent material and preparation method thereof.
Background technology：
Current commercial light source largely needs to use fluorescent material to make light conversion, the fluorescence prepared by rare-earth trichromatic fluorescent powder
Lamp is very energy-efficient new type light source, is the prior development direction of world's lighting source.China is all kinds of rare earth luminous at present
For material production capacity up to ten thousand tons, 2009, China produces about 7200 tons of all kinds of fluorescent RE powders, rare-earth trichromatic fluorescent lamp altogether
Yield ranks first in the world more than 3,000,000,000.Three-color fluorescent lamp (electricity-saving lamp) accounts for the 75% of rare earth luminescent material, is to send out at present
One of main application fields of luminescent material, and due to three-color fluorescent lamp than incandescent lamp have the advantages that energy-conservation, the long-life, future
Incandescent lamp will be phased out, turns into the fresh combatants of lamp ornaments lighting industry.Rare-earth trichromatic fluorescent powder then possesses uv radiation stability
The advantages that performance is good, the sudden temperature of heat is high, its finished product rare-earth trichromatic fluorescent lamp has the characteristics of specular removal, low light attenuation, long-life.
Phosphate has compared with strong absorption band because its phonon energy is moderate in VUV-ultraviolet (VUV-UV) region, is adapted to rear-earth-doped hair
Light, and have the advantages that luminous efficiency is high, physical and chemical performance is stable, raw material is easy to get and it is cheap, preparation technology is simple,
With very high application value.Using phosphate as matrix, it is glimmering that incorporation rare earth ion as exciting agent can be prepared by RE phosphate
Light powder.From the research of conventional all kinds of system fluorescent material it is seen that, Eu3+It is to apply more feux rouges active ions, Tb3+Then
It is to apply more green glow active ions.Since the seventies of last century six, both at home and abroad to the fluorescence using phosphate as matrix
The exploration of powder is also constantly being carried out, and is prepared for a series of RE phosphate fluorescent material (LaPO available for different field4:Ce3+,
Tb3+、(Sr,Mg)2P2O7:Eu2+), and show good optical property.From the point of view of anion structure, wherein studying more
Using wider mainly around orthophosphates (PO4)nWith pyrophosphate (P2O7)nSeries, its matrix do not light in itself, but in vacuum
There is stronger absorption ultraviolet-near ultraviolet band, and this charge migration just between rare earth ion-coordination oxygen matches, can be effective
Transfer energy to the centre of luminescence, and radiate in the form of light.Most research work all surrounds in the field at present
Deployed based on the doping vario-property for having been reported compound, or a series of isostructural compoundses compared with mature substrate are ground
Study carefully, and the work for exploring New-type matrix material is then relatively rare.A kind of noval chemical compound is from being found to synthesis pure sample, its composition proportion
Need to explore determination by many experiments Deng all；In addition, and not all compound be suitable as fluorescent material host material, it is desirable to
It has good heat endurance (fluorescent material does not change in room temperature long-time performance used above) and chemical stability (fluorescent material
Do not decompose or be not easy and device reacts), to characteristics such as the strong visible light-transmissive height of UV Absorption, thus those skilled in the art
It is generally acknowledged that the process for exploring new host material is very difficult.
The content of the invention：
The purpose of the present invention aims to provide a kind of red or green single-phase RE phosphate phosphor material of new host material
Material, has good optical property, and can meet the requirement of three-color fluorescent lamp very well.
Another object of the present invention is to, there is provided the simple its preparation process of above-mentioned material.
Single-phase red or green rare-earth phosphate phosphor material the chemical formula of the present invention is Mg21-28(In1-xLnx)28- 34P42-48Oy, Ln=Eu or Tb, x, y are molal quantity, wherein x=0.02~0.11, y=168~199.
Inventor has found Mg by studying21-28(In1-xEux)28-34P42-48OyEffective excitation wavelength be located at 210~280nm
In the range of, for red fluorescence powder.Mg21-28(In1-xTbx)28-34P42-48OyEffective excitation wavelength be located at 210~280nm scopes
It is interior, for green emitting phosphor.
The present invention is also first by a kind of new phosphate matrix, for fluorescent material, matrix components expression formula Mg21-28In28- 34P42-48Oy(y=168~199).The crystal belongs to anorthic system, P-1 (No.2) space group.Mix a small amount of active ions Ln3+
(Ln=Eu or Tb) substitutes part In3+, you can red or green Mg is made21-28(In1-xLnx)28-34P42-48Oy(x=0.02~
0.11, y=168~199) fluorescent material.
The phosphate compounds of the present invention wherein contains phosphide element, therefore rare earth element is easy to pass through as Validation Counter
The mode that part substitutes phosphide element enters in parent lattice, thus the compound that the present invention is prepared can be used as fluorescent material to use
Host material；There is not been reported for obtained this magnesium Indium phosphate host material of the invention in the prior art.Utilize the present invention
Host material X-ray powder diffraction data, indexing carried out using Fullprof softwares, it is tiltedly brilliant to show that the material belongs to three
System, P-1 (No.2) space group.Inventor by host material of the present invention by comparing joint committee (ICDD) powder
Last diffraction data storehouse (PDF-4+2011) and Inorganic crystal structure database (ICSD) and the softwares of MDI jade 5.0, it may be determined that
Matrix of the present invention is a kind of brand-new compound of crystal structure that there is not been reported.
Polycrystal synthesis is carried out using wet-chemical-solid-phase sintering method in the present invention, detailed process is as follows：Because the fluorescence
Powder host material is a kind of new solid solution compound without reporting and structure is unknown, and its ideal linearity molecular formula is
Mg3In4P6O24, because therefore Mg/In/P mutually has certain solid solubility scope in lattice, its actual solid solution molecular formula
Mg21-28In28-34P42-48Oy。
When preparing fluorescent material sample using wet-chemical-solid phase reaction method, by Mg：(In1-xLnx)：P mol ratio is
(21~28)：(28~34)：(42~48) weigh appropriate MgO, In2O3(Eu2O3/Tb4O7) and NH4H2PO4It is put into beaker,
Strong acid (such as nitric acid) is added, heating stirring makes dissolution of raw material, and polyvinyl alcohol and deionized water, heating are added after solution clarification
Stirring to being evaporated completely, and grinding is uniform after drying；First stage sintering is carried out at 1100-1300 DEG C, room temperature is cooled to, grinds
Mill, second stage sintering is then carried out under 1100-1300 DEG C of temperature conditionss, cooled down, grinding, obtain final product.
In preparation process of the present invention, the heating rate of first stage sintering step is preferably 3~7 DEG C/min；
In preparation process of the present invention, the heating rate of second stage sintering step is preferably 3~7 DEG C/min；
In preparation process of the present invention, the soaking time of first stage sintering step is preferably 10~20 hours；
In preparation process of the present invention, the soaking time of second stage sintering step is preferably 10~20 hours.
The present invention XRD results show this method synthesis rare earth doping fluorescent powder sample crystal structure with it is undoped
Pure phase compared to not changing.
In specific research process, explored and determined according to many experiments, according to Mg：(In1-xLnx)：P mol ratios are (21
~28)：(28~34)：(42~48) weigh raw material MgO, In2O3(Eu2O3/Tb4O7) and NH4H2PO4, and according to the wet of the present invention
Chemistry-solid-phase synthesis preparation technology, the Mg of x=0.02~0.11 of the present invention can be obtained21-28(In1-xLnx)28-34P42- 48OyProduct.
Beneficial effects of the present invention
It is glimmering as the red and green of phosphor host that the present invention successfully explores a kind of new phosphate compounds
Light powder, and using magnesium Indium phosphate as the phosphor material powder of matrix, there is not been reported in the prior art；Fluorescence obtained by the present invention
Powder has in ultra-violet (UV) band Absorber Bandwidth (200~280nm wave-length coverages), it is seen that light area transmitance is high, and luminous intensity is high, stability
Well, the features such as preparation technology is simpler.
Two kinds of novel phosphoric acid salt base fluorescent powders that the present invention is prepared.Wherein Mg21-28(In1-xEux)28-34P42-48OyMost
Good excitation wavelength is located at 234nm or so, and most strong launch wavelength is located at 589nm and 599nm, meets electricity-saving lamp red fluorescence powder
Condition；Carrying out attenuation curve test analysis to such fluorescent material finds its fluorescence lifetime in 6.2ms or so.Mg21-28(In1- xTbx)28-34P42-48OyMaximum excitation wavelength is located at 228nm and 251nm or so, and most strong launch wavelength is located near 541nm, very well
Meet energy-conservation green-fluorescent powder for lamp condition；Attenuation curve test analysis is carried out to such fluorescent material and finds its fluorescence longevity
Life is in 7.3ms or so.The fluorescent material of the present invention is suitable in three-color fluorescent lamp.
Light-emitting phosphor intensity prepared by the present invention is high, the sunset glow time is short, can effectively be excited by 200~270nm light.Separately
Outside, preparation method of the invention needs the equipment used and synthesis technique simple, is suitable for large-scale industrial production, these features
Just the requirement of three-color fluorescent lamp is met.
Brief description of the drawings：
Fig. 1 is embodiment 1, and comparative example 1-3 XRD spectrum compares；
In Fig. 1 it is unmarked go out the corresponding present invention of diffraction maximum Mg21-28In28-34P42-48OyDiffraction maximum.Can from figure
Go out, embodiment 1, contain Mg in the sample XRD spectrum obtained by comparative example 1-321-28In28-34P42-48OyDiffraction maximum, comparative example
Product made from 1~comparative example 3 is mixed phase, and the product obtained by embodiment 1 is Mg in the present invention21-28In28-34P42-48Oy
The single phase composition sample of phosphor host.
Fig. 2 is embodiment 1, embodiment 2, the XRD spectrum of 3 three samples of embodiment compare；
It can be seen that sample XRD spectrum made from embodiment 2, embodiment 3 and the sample XRD spectrum of embodiment 1 are complete
It is complete consistent, occur without miscellaneous peak, be Mg in the present invention21-28In28-34P42-48OyThe single phase composition sample of phosphor host
Product.
Fig. 3 is embodiment 1, embodiment 4, and 7 three sample XRD spectrums of embodiment compare；
Product made from embodiment 1 is single-phase, and all diffraction maximums belong to Mg in its XRD spectrum21-28In28-34P42-48Oy。
As shown in Figure 1, embodiment 4, the position consistency of the diffraction maximum and the diffraction maximum of embodiment 1 of product obtained by embodiment 7, and do not have
Miscellaneous peak occurs, it is known that the product obtained by embodiment 4, embodiment 7 is single-phase.
Fig. 4 is Mg made from embodiment 4~621-28(In1-xEux)28-34P42-48OyThe exciting light spectrogram of fluorescent material；
It is 598nm by fixed transmission wavelength, measures the excitation spectrum of fluorescent material made from embodiment 4~6, can from figure
To find out, occur in the range of 200~500nm at 200-280nm, 316nm, 360nm, 380nm, 392nm and 463nm
Excitation peak, wherein the width in the range of 200-280nm excites peak intensity to be significantly stronger than other excitation peaks；It is obvious that implement
The intensity of fluorescent material PLE made from example 4 is higher than fluorescent material made from embodiment 5 and 6.
Fig. 5 is Mg made from embodiment 4~621-28(In1-xEux)28-34P42-48OyThe launching light spectrogram of fluorescent material；
According to the excitation peak feature of embodiment in Fig. 4 4~6, fixed excitation wavelength is 234nm, and measurement embodiment 4~6 is made
Fluorescent material emission spectrum, it can be seen that in the range of 525~720nm positioned at 590nm, 599nm, 609nm,
Occurs emission peak at 614nm, 623nm, 651nm, 660nm, 687nm and 707nm, the transmitting peak intensity at 595nm is obvious
It is better than other positions diffraction maximum；It is made it is obvious that the intensity that phosphor emission made from embodiment 4 is composed is higher than embodiment 5 and 6
Fluorescent material.
Wherein, requirement of the three-color fluorescent lamp to fluorescent material be：Maximum excitation wavelength is in 254nm or so.According to Fig. 4 and figure
5 understand that fluorescent material made from embodiment 4~6 can apply to the red color components of three-color fluorescent lamp.
Mg made from Fig. 6 embodiments 7~921-28(In1-xTbx)28-34P42-48OyThe exciting light spectrogram of fluorescent material；
It is 541nm by fixed Tb characteristic emission wavelengths, measures the excitation spectrum of fluorescent material made from embodiment 7~9, from
It can be seen from the figure that, occur in the range of 200~500nm at 200~237nm, 237~285nm and 330~386nm
Excitation peak, wherein the width in the range of 200~285nm excites peak intensity to be significantly stronger than other excitation peaks；It is obvious that implement
The intensity of fluorescent material PLE made from example 7 is higher than fluorescent material made from embodiment 8 and 9.
Fig. 7 is Mg made from embodiment 7~921-28(In1-xEux)28-34P42-48OyThe launching light spectrogram of fluorescent material；
It is 228nm to fix excitation wavelength according to the excitation peak of embodiment in Fig. 6 7~9, measures fluorescence made from embodiment 7~9
The emission spectrum of powder, it can be seen that in the range of 350~680nm positioned at 378nm, 411nm, 437nm, 490nm,
Occurs emission peak at 500nm, 541nm, 548nm, 585nm, 599nm and 624nm, the emission peak at 541nm is highest peak；
It is obvious that the intensity that phosphor emission made from embodiment 7 is composed is higher than fluorescent material made from embodiment 8 and 9.
Wherein, requirement of the three-color fluorescent lamp to fluorescent material be：Maximum excitation wavelength is in 254nm or so.According to Fig. 6 and figure
7 understand that fluorescent material made from embodiment 4~6 can apply to the green components of three-color fluorescent lamp.
Fig. 8 is embodiment 4, the chromaticity coordinate figure of fluorescent material made from embodiment 7；
Chromaticity coordinate analysis is carried out to the fluorescent material using cie color software, determines embodiment 4, the chromaticity coordinate of embodiment 7
Respectively (0.6167,0.3827), (0.3050,0.5506).
Fig. 9 is the fluorescence lifetime curve of fluorescent material made from embodiment 4；
By carrying out fluorescence lifetime test to the fluorescent material, circle represents experiment value in figure, and solid line is fitting data, fitting
Data fit formula y=A1*exp(-x/t1)+y0, the fluorescence lifetime for calculating fluorescent material is 6.252ms.
Figure 10 is the fluorescence lifetime curve of fluorescent material made from embodiment 7；
By carrying out fluorescence lifetime test to the fluorescent material, circle represents experiment value in figure, and solid line is fitting data, fitting
Data fit formula y=A1*exp(-x/t1)+A2*exp(-x/t2)+y0, pass through weighted formula τ=(A1*t1 2+A2*t2 2)/(A1*
t1+A2*t2), the fluorescence lifetime for calculating fluorescent material is 7.302ms.
Figure 11 is embodiment 1, the XRD spectrum of 4 two samples of comparative example compares；
The sample of synthetic example 4 outside given composition section, there is Mg in its XRD diffraction spectra3P2O8Second phase, table
It is bright to synthesize Mg outside given composition section21-28In28-34P42-48OySingle-phase sample.
Figure 12 is embodiment 7, the launching light spectrogram of the obtained fluorescent material of 5 two samples of comparative example
It can be evident that from figure, the intensity that phosphor emission made from embodiment 7 is composed is higher than comparative example 5 and made
The fluorescent material obtained.
Embodiment：
The present invention is intended to further illustrate with reference to embodiments, is not intended to limit the present invention.
Embodiment 1：Mg25In30P45O182.5The preparation of fluorescent material matrix
Weigh 0.1947g MgO, 0.8049g In2O3、1.0004g NH4H2PO4It is placed in beaker, adding appropriate nitric acid makes
Dissolution of raw material, a small amount of polyvinyl alcohol and appropriate amount of deionized water are added after solution clarification, heating stirring puts beaker to being evaporated completely
Ground after being dried in drying box uniform；Two steps are carried out afterwards burns (1200 DEG C of first stage sintering temperature, after being incubated 15 hours eventually
With room temperature is furnace-cooled to, grind 10 minutes；1200 DEG C of second stage sintering temperature, insulation cool to room temperature with the furnace after 15 hours, and two
Step sintering heating rate is 5 DEG C/min).Burned sample is taken out and ground, you can Mg is made25In30P45O182.5Fluorescent material
Matrix.Through indexing, its cell parameter is：α=104.4420 °,
109.8360 °, γ=100.3720 °,Z=1.
Embodiment 2：Mg23In29P44O176.5The preparation of fluorescent material matrix
Weigh 0.1851g MgO, 0.8040g In2O3、1.0108g NH4H2PO4, remaining step is same as Example 1.
Embodiment 3：Mg27In33P47O194The preparation of fluorescent material matrix
Weigh 0.1965g MgO, 0.8272g In2O3、0.9763g NH4H2PO4, remaining step is same as Example 1.
Embodiment 4：Mg25(In0.98Eu0.02)30P45O182.5The preparation of fluorescent material
Weigh 0.1943g MgO, 0.7871g In2O3、0.0204g Eu2O3、0.9982g NH4H2PO4, remaining step with
Embodiment 1 is identical.
Embodiment 5：Mg25(In0.95Eu0.05)30P45O182.5The preparation of fluorescent material
Weigh 0.1937g MgO, 0.7605g In2O3、0.0507g Eu2O3、0.9950g NH4H2PO4, remaining step with
Embodiment 1 is identical.
Embodiment 6：Mg25(In0.91Eu0.09)30P45O182.5The preparation of fluorescent material
Weigh 0.1929g MgO, 0.7254g In2O3、0.0909g Eu2O3、0.9908g NH4H2PO4, remaining step with
Embodiment 1 is identical.
Embodiment 7：Mg25(In0.93Tb0.07)30P45O182.5The preparation of fluorescent material
Weigh 0.1929g MgO, 0.7413g In2O3、0.0751g Tb4O7、0.9907g NH4H2PO4, remaining step with
Embodiment 1 is identical.
Embodiment 8：Mg25(In0.95Tb0.05)30P45O182.5The preparation of fluorescent material
Weigh 0.1934g MgO, 0.7593g In2O3、0.0538g Tb4O7、0.9935g NH4H2PO4, remaining step with
Embodiment 1 is identical.
Embodiment 9：Mg25(In0.91Tb0.09)30P45O182.5The preparation of fluorescent material
Weigh 0.1923g MgO, 0.7234g In2O3、0.0963g Tb4O7、0.9880g NH4H2PO4, remaining step with
Embodiment 1 is identical.
Comparative example 1：Mg：In：P mol ratios are 33.3：22.2：The preparation of 44.5 sample
Weigh 0.2816g MgO, 0.6467g In2O3、1.0717g NH4H2PO4, remaining step is same as Example 1.
Comparative example 2：Mg：In：P mol ratios are 23：37：The preparation of 40 sample
Weigh 0.1739g MgO, 0.9633g In2O3、0.8629g NH4H2PO4, remaining step is same as Example 1.
Comparative example 3：Mg：In：P mol ratios are 30：28：The preparation of 42 sample
Weigh 0.2436g MgO, 0.7831g In2O3、0.9733g NH4H2PO4, remaining step is same as Example 1.
Comparative example 4：(outside the given composition range scope of the present invention) Mg30In28P42O177The preparation of sample
Weigh 0.2413g MgO, 0.7757g In2O3、0.9642g NH4H2PO4, remaining step is same as Example 1.
Comparative example 5：(outside the given composition range scope of the present invention) Mg30(In0.93Tb0.07)28P42O177The preparation of sample
Weigh 0.2413g MgO, 0.7214g In2O3、0.0731g Tb4O7、0.9642g NH4H2PO4, remaining step with
Embodiment 1 is identical.
Claims (10)
1. a kind of red or green rare-earth phosphate phosphor material, it is characterised in that its chemical formula is Mg21-28(In1- xLnx)28-34P42-48OySingle-phase phosphor material powder, wherein Ln=Eu or Tb, x, y are molal quantity, wherein x=0.02~0.11, y=
168~199.
2. a kind of RE phosphate phosphor material powder according to claim 1, it is characterised in that the fluorescent material is with phosphoric acid
Salt Mg21-28In28-34P42-48OyFor matrix, wherein y is molal quantity, y=168~199, passes through 0.02~0.11 mole of Eu of incorporation3+
Or Tb3+Into In3+Position, is obtained.
A kind of 3. RE phosphate phosphor material powder according to claim 2, it is characterised in that the phosphate Mg21- 28In28-34P42-48OyMatrix belongs to anorthic system,Space group.
A kind of 4. RE phosphate phosphor material powder according to claim 1, it is characterised in that Mg21-28(In1- xEux)28-34P42-48OyEffective excitation wavelength be located in the range of 210~280nm, for red fluorescence powder.
A kind of 5. RE phosphate phosphor material powder according to claim 1, it is characterised in that Mg21-28(In1- xTbx)28-34P42-48OyEffective excitation wavelength be located in the range of 210~280nm, for green emitting phosphor.
6. the preparation method of the RE phosphate phosphor material powder described in claim any one of 1-5, it is characterized in that：According to chemistry
Formula is Mg21-28(In1-xLnx)28-34P42-48OyRequired nonstoichiometric molar ratio weighs MgO, In2O3、Eu2O3Or Tb4O7And
NH4H2PO4, it is placed in beaker, adding nitric acid makes dissolution of raw material, adds polyvinyl alcohol after solution clarification and deionized water, heating are stirred
Mix to being evaporated completely, material grinding is uniform after drying；First stage sintering is carried out at 1100-1300 DEG C, room temperature is cooled to, grinds
Mill, second stage sintering is then carried out under 1100-1300 DEG C of temperature conditionss, ground after cooling and obtain final product.
7. the preparation method of RE phosphate base fluorescent powder material according to claim 6, it is characterised in that first stage
The heating rate of sintering is 3~7 DEG C/min.
8. the preparation method of RE phosphate base fluorescent powder material according to claim 6, it is characterised in that second stage
The heating rate of sintering is 3~7 DEG C/min.
9. the preparation method of phosphate base phosphor material powder according to claim 6, it is characterised in that the first stage sinters
10~20h of soaking time.
10. the preparation method of phosphate base phosphor material powder according to claim 6, it is characterised in that second stage is burnt
10~20h of soaking time of knot.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1082090A (en) * | 1993-08-06 | 1994-02-16 | 上海跃龙有色金属有限公司 | High-performance phosphate green emitting phosphor and manufacture method thereof |
| JP2001308382A (en) * | 2000-04-25 | 2001-11-02 | Nippon Telegr & Teleph Corp <Ntt> | Light-emitting element |
| CN101372760A (en) * | 2008-09-10 | 2009-02-25 | 太原理工大学 | Preparation of glowing oxygen doped gallium arsenide polycrystalline film |
| CN103911600A (en) * | 2014-04-21 | 2014-07-09 | 电子科技大学 | Preparation method of InP thin-film material |
| CN104449721A (en) * | 2013-09-25 | 2015-03-25 | 海洋王照明科技股份有限公司 | Europium dysprosium co-doping rare earth phosphorus indium acid salt light-emitting film as well as preparation method and application of europium dysprosium co-doping rare earth phosphorus indium acid salt light-emitting film |
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| KR930005691B1 (en) * | 1990-02-28 | 1993-06-24 | 삼성전관 주식회사 | Red-luminous phosphor |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1082090A (en) * | 1993-08-06 | 1994-02-16 | 上海跃龙有色金属有限公司 | High-performance phosphate green emitting phosphor and manufacture method thereof |
| JP2001308382A (en) * | 2000-04-25 | 2001-11-02 | Nippon Telegr & Teleph Corp <Ntt> | Light-emitting element |
| CN101372760A (en) * | 2008-09-10 | 2009-02-25 | 太原理工大学 | Preparation of glowing oxygen doped gallium arsenide polycrystalline film |
| CN104449721A (en) * | 2013-09-25 | 2015-03-25 | 海洋王照明科技股份有限公司 | Europium dysprosium co-doping rare earth phosphorus indium acid salt light-emitting film as well as preparation method and application of europium dysprosium co-doping rare earth phosphorus indium acid salt light-emitting film |
| CN103911600A (en) * | 2014-04-21 | 2014-07-09 | 电子科技大学 | Preparation method of InP thin-film material |
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