CN103205253A - Columbate or tantalate fluorescence material used in white-light LED, and its preparation method - Google Patents
Columbate or tantalate fluorescence material used in white-light LED, and its preparation method Download PDFInfo
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- CN103205253A CN103205253A CN2012105276199A CN201210527619A CN103205253A CN 103205253 A CN103205253 A CN 103205253A CN 2012105276199 A CN2012105276199 A CN 2012105276199A CN 201210527619 A CN201210527619 A CN 201210527619A CN 103205253 A CN103205253 A CN 103205253A
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- tantalite
- fluorescent material
- white light
- light leds
- niobate
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
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Abstract
The invention relates to a columbate or tantalate fluorescence material used in white-light LED, and its preparation method. The columbate or tantalate fluorescence material comprises undoped columbate or tantalite, transition metal doped columbate or tantalite, Tl-like ion doped columbate or tantalite having an s<2> configuration, rare earth element doped columbate or tantalite, and Tl-like ion and rare earth ion co-doped columbate or tantalite. The material can be used in the white-light LED, and relevant display and illumination devices. The columbate or tantalate fluorescence material has the advantages of cheap and easily available raw materials, simple preparation technology, stable chemical properties, and excellent luminescence performance, and is an ideal phosphor candidate material for the white-light LED.
Description
Technical field
The present invention relates to belong to the fluorescent material field for the niobate of white light LEDs or tantalite fluorescent material and preparation method thereof.
Background technology
White light LEDs be after incandescent light, fluorescent lamp and electricity-saving lamp the 4th generation lighting electric light source, or be called the 21 century green light source, have environmental protection, overlong service life, energy-efficient, anti-adverse environment, simple in structure, volume is little, in light weight, response is fast, operating voltage is low and the good characteristics of security.Substituting the traditional lighting light source with the LED solid state light emitter is present lighting engineering main development tendency, and each state all pays close attention, and has formulated evolutionary operation(EVOP) one after another, steps up development and exploitation.
At present, the technology of preparing from light LED mainly comprises three kinds: light transformation approach, polychrome combined method and Multiple Quantum Well method.The light transformation approach namely adopts light-converting material, and purple light or blue light conversion are produced white light.The polychrome combined method is by the different indigo plant of emission wavelength, the green and compound white light of ruddiness combined transmit, and this scheme is to the circuit requirement height, and is difficult for obtaining stable white light source when power-supply fluctuation or temperature variation.The Multiple Quantum Well method is the diode that directly preparation emits white light, and it is ripe that is that all right technically at present.
The light transformation approach is present the most ripe technical method.According to luminescence and colorimetry principle, mainly comprise following scheme:
(1) blue led chip and the jaundice emitting phosphor that can effectively be excited by blue light are in conjunction with forming white light LEDs.The blue chip emission of semiconductor compound blue light belongs to the p-n junction electroluminescent.Part blue light is absorbed by fluorescent material, and excitated fluorescent powder emission gold-tinted belongs to typical converting photoluminescent down.Gold-tinted and the remaining blue light of emission are regulated and control their strength ratio, can obtain the white light of various colour temperatures.Certainly, also can add can blue-light excited be glowed, green light fluorescent powder obtains white light.This principle and scheme are the main flows of current development.The most typical scheme of this principle is turn blue light for InGaN chip and the Ce that scribbles jaundice light
3+Activate (Y, Gd)
3(Al, Ga)
5O
12White light LEDs, commercialization are formed in the encapsulation of yttrium aluminum garnet yellow fluorophor.This technical scheme exists that color developing is poor, colour temperature is higher, lacks the shortcoming of red composition, needs to add and can be improved performance by blue-light excited red fluorescence powder.
(2) the ultraviolet leds chip is launched red, green, blue three-color phosphor combination composition white light LEDs with can effectively being excited by this UV-light.The similar three primary colours compact fluorescent lamp of its principle can select for use multiple fluor to cooperate.The characteristics of scheme are that the kind that the high-efficiency fluorescence body is selected is enriched, and can obtain light efficiency height, colour rendering index height and various correlated(color)temperatures, and are alternative strong.But also there is the low problem of fluorescent material efficiency of conversion in this scheme.
Therefore, synthetic have good luminous characteristic, chemical property is stable, cost is low New LED is most important to the white light LEDs of realizing high brightness with fluorescent material, especially the red fluorescence powder of excellent property lacks very much.The excitation spectrum of many materials sharply descends in the 380-410nm scope, blue light region do not have excite or intensity very low.As Y
2O
3: Eu, it excites down at 254nm is most effective red-emitting phosphors, but long wave UV and blue-light excited invalid substantially.Equally, colour TV Y
2O
2The S:Eu fluorescent material has similar problem.
At present, the fluorescent material system of people's broad research concentrates on phosphoric acid salt (as rare-earth activated lanthanum orthophosphate), borate mostly (as (Y, Gd) BO
3: Eu rouge and powder), aluminate is (as BaMgAl
10O
17: Eu blue powder), silicate is (as Zn
2SiO
4: the green powder of Mn), oxide compound is (as red fluorescence powder Y
2O
3: Eu) etc.People are also fewer to the research report of niobate, tantalate material.Niobate, tantalate material category are various, and structure is different, has constituted a wide band gap semiconducter family, and it is cheap, is potential good luminous host material.
Summary of the invention
First purpose of the present invention is the technical characterstic in the past, proposes a kind of niobate or tantalite fluorescent material for white light LEDs.
For realizing first purpose of the present invention, one of the solution of the present invention is, a kind of niobate or tantalite fluorescent material for white light LEDs, and chemical formula is A
aM
bM '
cO
d, wherein:
A is one or more in second main group element, one or more among preferred Ca, Sr or the Ba;
M is one or more in the 3rd main group element or Sc or Y or the lanthanide series rare-earth elements, one or more among preferred Al, Ga, In, Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb or the Lu;
M ' is a kind of among Nb or the Ta;
0＜a≤2，0＜b≤3，0＜c≤3，0＜d≤14。
This type of fluorescent material shows the feature emission of corresponding rare earth ion in its component, as Ca
2EuNbO
6And Sr
2EuNbO
6Show Eu respectively
3+The red emission of ion and orange red light emission, this type of fluorescent material includes but not limited to:
Ca
2EuNbO
6, Ca
2EuTaO
6, Sr
2EuNbO
6, Sr
2EuTaO
6, Ba
2EuNbO
6, Ba
2EuTaO
6, (Ca
0.1Sr
0.9)
2EuNbO
6, (Ca
0.1Sr
0.9)
2EuTaO
6, (Sr
0.2Ba
0.8)
2EuNbO
6, (Sr
0.2Ba
0.8)
2EuTaO
6, Ca
2TbNbO
6, Ca
2TbTaO
6, Ba
2SmNbO
6, Ba
2SmTaO
6, Ca
2Eu
3Nb
3O
14, Ca
2Eu
3Ta
3O
14, Ca
2Pr
3Nb
3O
14, Ca
2Pr
3Ta
3O
14Deng
For realizing first purpose of the present invention, one of the solution of the present invention is, a kind of niobate or tantalite fluorescent material for white light LEDs, and chemical formula is A
aM
bM '
cO
d: M
I x, wherein:
A is one or more in second main group element, one or more among preferred Ca, Sr or the Ba;
M is one or more in the 3rd main group element or Sc or Y or the lanthanide series rare-earth elements, one or more among preferred Al, Ga, In, Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb or the Lu;
M ' is a kind of among Nb or the Ta;
M
IBe in the transition metal one or more, one or more among preferred Cu, Mn, Cr or the Ag;
0＜a≤2，0＜b≤3，0＜c≤3，0＜d≤14，0＜x≤0.5。
This type of fluorescent material can realize comprising the VISIBLE LIGHT EMISSION of ruddiness, includes but not limited to:
Ca
2YNbO
6: 0.01Mn, Ca
2YTaO
6: 0.01Mn, Ca
2GdNbO
6: 0.01Mn, Ca
2GdTaO
6: 0.01Mn, Ca
2LaNbO
6: 0.01Mn, Ca
2LaTaO
6: 0.01Mn, Ca
2La
3Nb
3O
14: 0.01Mn, Ca
2La
3Ta
3O
14: 0.01Mn, Ca
2Y
3Nb
3O
14: 0.01Mn, Ca
2Y
3Ta
3O
14: 0.01Mn etc.
For realizing first purpose of the present invention, one of the solution of the present invention is, a kind of niobate or tantalite fluorescent material for white light LEDs, and chemical formula is A
aM
bM '
cO
d: M
II x, wherein:
A is one or more in second main group element, one or more among preferred Ca, Sr or the Ba;
M is one or more in the 3rd main group element or Sc or Y or the lanthanide series rare-earth elements, one or more among preferred Al, Ga, In, Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb or the Lu;
M ' is a kind of among Nb or the Ta;
M
IIBe to be selected to have s
2In the class Tl ion of configuration one or more, one or more among preferred Bi, Sb, Pb or the Sn;
0＜a≤2，0＜b≤3，0＜c≤3，0＜d≤14，0＜x≤0.5。
This type of fluorescent material can be realized blue emission, includes but not limited to:
Ca
2YNbO
6: 0.01Bi, Ca
2YTaO
6: 0.01Bi, Ca
2GdNbO
6: 0.01Bi, Ca
2GdTaO
6: 0.01Bi, Ca
2LaNbO
6: 0.01Bi, Ca
2LaTaO
6: 0.01Bi, Ca
2(La
0.9Y
0.1) NbO
6: 0.01Bi, Ca
2(La
0.9Y
0.1) TaO
6: 0.01Bi, (Ca
0.1Sr
0.9)
2LaNbO
6: 0.01Bi, (Ca
0.1Sr
0.9)
2LaTaO
6: 0.01Bi, (Sr
0.1Ba
0.9)
2(Y
0.1La
0.9) NbO
6: 0.01Bi, (Sr
0.1Ba
0.9)
2(Y
0.1La
0.9) TaO
6: 0.01Bi, Ca
2La
3Nb
3O
14: 0.01Bi, Ca
2La
3Ta
3O
14: 0.01Bi, Ca
2Y
3Nb
3O
14: 0.01Bi, Ca
2Y
3Ta
3O
14: 0.01Bi, Sr
2GdNbO
6: 0.01Bi, Sr
2GdTaO
6: 0.01Bi etc.
For realizing first purpose of the present invention, one of the solution of the present invention is, a kind of niobate or tantalite fluorescent material for white light LEDs, and chemical formula is A
aM
bM '
cO
d: M
III x, wherein:
A is one or more in second main group element, one or more among preferred Ca, Sr or the Ba;
M is one or more in the 3rd main group element or Sc or Y or the lanthanide series rare-earth elements, one or more among preferred Al, Ga, In, Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb or the Lu;
M ' is a kind of among Nb or the Ta;
M
IIIBe in the rare earth element one or more, one or more among preferred Ce, Pr, Nd, Sm, Eu, Tb, Dy, Ho, Er, Tm or the Yb;
0＜a≤2，0＜b≤3，0＜c≤3，0＜d≤14，0＜x≤5。
This type of fluorescent material shows the visible light intensity emission of corresponding rare earth ion doped feature, as Ca
2LaSbO
6: 0.5Eu has strong red emission, and this type of fluorescent material includes but not limited to:
Ca
2LaNbO
6: 0.5Eu, Ca
2LaTaO
6: 0.5Eu, Ca
2YNbO
6: 0.5Eu, Ca
2YTaO
6: 0.5Eu, Ca
2GdNbO
6: 0.5Eu, Ca
2GdTaO
6: 0.5Eu, Ca
2(Y
0.1La
0.9) NbO
6: 0.5Eu, Ca
2(Y
0.1La
0.9) TaO
6: 0.5Eu, Sr
2GdNbO
6: 0.3Eu, Sr
2GdTaO
6: 0.3Eu, Ba
2LaNbO
6: 0.1Eu, Ba
2LaTaO
6: 0.1Eu, (Sr
0.1Ba
0.9)
2YNbO
6: 0.5Eu, (Sr
0.1Ba
0.9)
2YTaO
6: 0.5Eu, Ca
2La
3Nb
3O
14: 0.1Eu, Ca
2La
3Ta
3O
14: 0.1Eu, Ca
2Y
3Nb
3O
14: 0.1Eu, Ca
2Y
3Ta
3O
14: 0.1Eu, Ca
2Gd
3Nb
3O
14: 0.1Eu, Ca
2Gd
3Ta
3O
14: 0.1Eu, Sr
2Gd
3Nb
3O
14: 0.1Eu, Sr
2Gd
3Ta
3O
14: 0.1Eu, Ca
2LaNbO
6: 0.1Ce, Ca
2LaTaO
6: 0.1Ce, Ca
2YNbO
6: 0.1Pr, Ca
2YTaO
6: 0.1Pr, Ca
2GdNbO
6: 0.1Tb, Ca
2GdTaO
6: 0.1Tb, Sr
2GdNbO
6: 0.1Sm, Sr
2GdTaO
6: 0.1Sm, Ca
2La
3Nb
3O
14: 0.1Ce, Ca
2La
3Ta
3O
14: 0.1Ce, Ca
2Y
3Nb
3O
14: 0.1Tb, Ca
2Y
3Ta
3O
14: 0.1Tb, Ca
2Gd
3Nb
3O
14: 0.1Pr, Ca
2Gd
3Ta
3O
14: 0.1Pr, Sr
2Gd
3Nb
3O
14: 0.1Sm, Sr
2Gd
3Ta
3O
14: 0.1Sm, Ca
2YNbO
6: 0.1Tb, 0.2Eu, Ca
2YTaO
6: 0.1Tb, 0.2Eu, Ca
2LaNbO
6: 0.1Ce, 0.2Eu, Ca
2LaTaO
6: 0.1Ce, 0.2Eu, Ca
2YNbO
6: 0.1Ce, 0.1Tb, Ca
2YTaO
6: 0.1Ce, 0.1Tb etc.
For realizing first purpose of the present invention, one of the solution of the present invention is, a kind of niobate or tantalite fluorescent material for white light LEDs, and chemical formula is A
aM
bM '
cO
d: M
II yM
III z, wherein:
A is one or more in second main group element, one or more among preferred Ca, Sr or the Ba;
M is one or more in the 3rd main group element or Sc or Y or the lanthanide series rare-earth elements, one or more among preferred Al, Ga, In, Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb or the Lu;
M ' is a kind of among Nb or the Ta;
M
IIBe to be selected to have s
2In the class Tl ion of configuration one or more, one or more among preferred Bi, Sb, Pb or the Sn;
M
IIIBe in the rare earth element one or more, one or more among preferred Ce, Pr, Nd, Sm, Eu, Tb, Dy, Ho, Er, Tm or the Yb;
0＜a≤2，0＜b≤3，0＜c≤3，0＜d≤14，0＜y≤1，0＜z≤5。
This type of fluorescent material can be realized two bands or the emission more than two bands in same matrix.As Ca
2GdNbO
6: 0.005Bi, can observe blue emission band and red emission band simultaneously among the 0.2Eu, this type of fluorescent material includes but not limited to:
Ca
2GdNbO
6: 0.005Bi, 0.2Eu, Ca
2GdTaO
6: 0.005Bi, 0.2Eu, Ca
2LaNbO
6: 0.005Bi, 0.2Eu, Ca
2LaTaO
6: 0.005Bi, 0.2Eu, Ca
2YNbO
6: 0.005Bi, 0.2Tb, Ca
2YTaO
6: 0.005Bi, 0.2Tb etc.
The niobate or the tantalite fluorescent material that are used for white light LEDs of realizing the present invention's first purpose such scheme can possess arbitrary structures, include but not limited to perovskite structure, counterfeit perovskite structure, structure of double perovskite, olivine structural, pyrochlore structure; Wherein preferred structure is counterfeit perovskite structure, structure of double perovskite and pyrochlore structure; Structure of double perovskite more preferably.
Realize the niobate or the tantalite fluorescent material M that are used for white light LEDs of the present invention's first purpose such scheme
I, M
II, M
IIITransition metal, rare earth element, have s
2The class Tl ion of configuration depends on parent lattice strongly as its luminosity of luminescence center ion, by selecting suitable substrate material for it, regulates its coordinate crystal field, can regulate its glow color, the VISIBLE LIGHT EMISSION that obtains expecting.This three classes luminescence center ion and A
aM
bM '
cO
dCorresponding cationic radius in the substrate material, charge differences is little, can enter parent lattice easily, realizes high doping and strong luminous.
Second purpose of the present invention is to propose the preparation method of a kind of niobate for white light LEDs or tantalate fluorescence material.
For realizing second purpose of the present invention, one of the solution of the present invention comprises the steps:
Step (1): press chemical formula
A
aM
bM '
cO
dOr A
aM
bM '
cO
d: M
I xOr A
aM
bM '
cO
d: M
II xOr A
aM
bM '
cO
d: M
III xJoin and get raw material, wherein:
A is one or more in second main group element, one or more among preferred Ca, Sr or the Ba;
M is one or more in the 3rd main group element or Sc or Y or the lanthanide series rare-earth elements, one or more among preferred Al, Ga, In, Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb or the Lu;
M ' is a kind of among Nb or the Ta;
M
IBe in the transition metal one or more, one or more among preferred Cu, Mn, Cr or the Ag;
M
IIBe to be selected to have s
2In the class Tl ion of configuration one or more, one or more among preferred Bi, Sb, Pb or the Sn;
M
IIIBe in the rare earth element one or more, one or more among preferred Ce, Pr, Nd, Sm, Eu, Tb, Dy, Ho, Er, Tm or the Yb;
0＜a≤2，0＜b≤3，0＜c≤3，0＜d≤14，0＜x≤5。
Described raw material is the inorganic salt of each element, includes but not limited to oxide compound, carbonate, nitrate or acetate etc.
Step (2): with 1000～1700 ℃ of high-temperature calcinations under vacuum, air, oxygen, rare gas element or reducing gas environment of above-mentioned whole raw materials, the preferred reaction times is 12～72 hours.
After above-mentioned steps (2), the preferred further repeating step (2) of step (2) products therefrom repeatedly.
After above-mentioned steps (2), step (2) products therefrom is preferably further heat-treated under the reducing gas environment.
Second purpose of the present invention is to propose the preparation method of a kind of niobate for white light LEDs or tantalate fluorescence material.
For realizing second purpose of the present invention, one of the solution of the present invention comprises the steps:
Step (1): press chemical formula
A
aM
bM '
cO
dOr A
aM
bM '
cO
d: M
I xOr A
aM
bM '
cO
d: M
II xOr A
aM
bM '
cO
d: M
III xJoin and get raw material, wherein:
A is one or more in second main group element, one or more among preferred Ca, Sr or the Ba;
M is one or more in the 3rd main group element or Sc or Y or the lanthanide series rare-earth elements, one or more among preferred Al, Ga, In, Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb or the Lu;
M ' is a kind of among Nb or the Ta;
M
IBe in the transition metal one or more, one or more among preferred Cu, Mn, Cr or the Ag;
M
IIBe to be selected to have s
2In the class Tl ion of configuration one or more, one or more among preferred Bi, Sb, Pb or the Sn;
M
IIIBe in the rare earth element one or more, one or more among preferred Ce, Pr, Nd, Sm, Eu, Tb, Dy, Ho, Er, Tm or the Yb;
0＜a≤2，0＜b≤3，0＜c≤3，0＜d≤14，0＜x≤5。
Described raw material is the inorganic salt of each element, includes but not limited to oxide compound, carbonate, nitrate or acetate etc.
Step (2): with 500～750 ℃ of pre-burnings under vacuum, air, oxygen, rare gas element or reducing gas environment of above-mentioned whole raw materials, the preferred reaction times is 0.1～48 hour.
Step (3): with 1000～1700 ℃ of high-temperature calcinations under vacuum, air, oxygen, rare gas element or reducing gas environment of step (2) products therefrom, the preferred reaction times is 12～72 hours.
After above-mentioned steps (2), the preferred further repeating step (2) of step (2) products therefrom repeatedly.
After above-mentioned steps (3), the preferred further repeating step (3) of step (3) products therefrom repeatedly.
After above-mentioned steps (3), step (3) products therefrom is preferably further heat-treated under the reducing gas environment.
For realizing second purpose of the present invention, one of the solution of the present invention comprises the steps:
Step (1): press chemical formula
A
aM
bM '
cO
dOr A
aM
bM '
cO
d: M
I xOr A
aM
bM '
cO
d: M
II xOr A
aM
bM '
cO
d: M
III xJoin and get raw material, wherein:
A is one or more in second main group element, one or more among preferred Ca, Sr or the Ba;
M is one or more in the 3rd main group element or Sc or Y or the lanthanide series rare-earth elements, one or more among preferred Al, Ga, In, Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb or the Lu;
M ' is a kind of among Nb or the Ta;
M
IBe in the transition metal one or more, one or more among preferred Cu, Mn, Cr or the Ag;
M
IIBe to be selected to have s
2In the class Tl ion of configuration one or more, one or more among preferred Bi, Sb, Pb or the Sn;
M
IIIBe in the rare earth element one or more, one or more among preferred Ce, Pr, Nd, Sm, Eu, Tb, Dy, Ho, Er, Tm or the Yb;
0＜a≤2，0＜b≤3，0＜c≤3，0＜d≤14，0＜x≤5。
Described raw material is the inorganic salt of each element, includes but not limited to oxide compound, carbonate, nitrate or acetate etc.
Step (2): with raw material 1000～1700 ℃ of high-temperature calcinations under vacuum, air, oxygen, rare gas element or reducing gas environment of described A and M and M ' element correspondence, the preferred reaction times is 12～72 hours.
Step (3): in step (2) products therefrom, add described M
IOr M
IIOr M
IIIOr (M
IAnd M
II) raw material 1000～1700 ℃ of high-temperature calcinations under vacuum, air, oxygen, rare gas element or reducing gas environment of element correspondence, the preferred reaction times is 12～72 hours.
After above-mentioned steps (2), the preferred further repeating step (2) of step (2) products therefrom repeatedly.
After above-mentioned steps (3), the preferred further repeating step (3) of step (3) products therefrom repeatedly.
After above-mentioned steps (3), step (3) products therefrom is preferably further heat-treated under the reducing gas environment.
For realizing second purpose of the present invention, one of the solution of the present invention comprises the steps:
Step (1): press chemical formula
A
aM
bM '
cO
dOr A
aM
bM '
cO
d: M
I xOr A
aM
bM '
cO
d: M
II xOr A
aM
bM '
cO
d: M
III xJoin and get raw material, wherein:
A is one or more in second main group element, one or more among preferred Ca, Sr or the Ba;
M is one or more in the 3rd main group element or Sc or Y or the lanthanide series rare-earth elements, one or more among preferred Al, Ga, In, Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb or the Lu;
M ' is a kind of among Nb or the Ta;
M
IBe in the transition metal one or more, one or more among preferred Cu, Mn, Cr or the Ag;
M
IIBe to be selected to have s
2In the class Tl ion of configuration one or more, one or more among preferred Bi, Sb, Pb or the Sn;
M
IIIBe in the rare earth element one or more, one or more among preferred Ce, Pr, Nd, Sm, Eu, Tb, Dy, Ho, Er, Tm or the Yb;
0＜a≤2，0＜b≤3，0＜c≤3，0＜d≤14，0＜x≤5。
Described raw material is the inorganic salt of each element, includes but not limited to oxide compound, carbonate, nitrate or acetate etc.
Step (2): with raw material 500～750 ℃ of pre-burnings under vacuum, air, oxygen, rare gas element or reducing gas environment of described A and M and M ' element correspondence, the preferred reaction times is 0.1～48 hour.
Step (3): with 1000～1700 ℃ of high-temperature calcinations under vacuum, air, oxygen, rare gas element or reducing gas environment of step (2) products therefrom, the preferred reaction times is 12～72 hours.
Step (4): in step (3) products therefrom, add described M
IOr M
IIOr M
IIIOr (M
IAnd M
II) raw material 1000～1700 ℃ of high-temperature calcinations under vacuum, air, oxygen, rare gas element or reducing gas environment of element correspondence, the preferred reaction times is 12～72 hours.
After above-mentioned steps (2), the preferred further repeating step (2) of step (2) products therefrom repeatedly.
After above-mentioned steps (3), the preferred further repeating step (3) of step (3) products therefrom repeatedly.
After above-mentioned steps (3), the preferred further repeating step (3) of step (4) products therefrom repeatedly.
After above-mentioned steps (4), step (4) products therefrom is preferably further heat-treated under the reducing gas environment.
Realize the niobate that is used for white light LEDs of the present invention's second purpose such scheme or the preparation method of tantalate fluorescence material, the preferred vacuum sealing by fusing of described vacuum environment silica tube.
Use the U-3010 spectrophotometric instrument of HIT to test its uv-visible absorption spectra to gained sample of the present invention; Use Shimadzu RF-5301PC fluorescence spectrophotometer to test its photoluminescence spectrum in gained sample of the present invention; Use French Flurolog-3 fluorescence spectrophotometer and Britain's FLS920 fluorescence spectrophotometer to test its photoluminescence life-span in gained sample of the present invention.
Luminescent material provided by the present invention can be by the optical excitation of various wavelength such as ultraviolet, near ultraviolet, blue light, and the emission band of luminescent material comprises various bands of a spectrum such as blue light, gold-tinted, ruddiness.
Luminous host material provided by the present invention has changeable crystalline structure and adjustable crystal field strength, simultaneously, the substrate material that provides also has broad-band gap and low charge transport characteristic, thereby can realize the luminescent material emission wavelength cut out effective optimization with luminosity continuously, especially for being difficult to realize high efficiency red light material, the invention provides broad selection space.
Description of drawings
Fig. 1 is the Ca that do not mix among the embodiment
2EuNbO
6Emission spectrum (the λ of material
Ex=464nm) and excitation spectrum (λ
Em=612nm).
Fig. 2 is Ca among the embodiment
2Y
1-xNbO
6: the emission spectrum (λ of xEu (x=0.05,0.3,0.75) material
Ex=464nm) and excitation spectrum (λ
Em=613nm).
Fig. 3 is Ca among the embodiment
2La
1-xNbO
6: the emission spectrum (λ of xEu (x=0.05,0.4,0.75) material
Ex=464nm) and excitation spectrum (λ
Em=613nm).
Fig. 4 is Ca among the embodiment
2Gd
1-xNbO
6: the emission spectrum (λ of xEu (x=0.05,0.5,0.75) material
Ex=464nm) and excitation spectrum (λ
Em=613nm).
Fig. 5 is Ca among the embodiment
2Y
0.7NbO
6: 0.3Eu, Ca
2Gd
0.7NbO
6: 0.3Eu, Ca
2La
0.7NbO
6: the emission spectrum (λ of 0.3Eu material
Ex=464nm) and excitation spectrum (λ
Em=613nm).
Fig. 6 is Sr among the embodiment
2Gd
0.7TaO
6: the emission spectrum (λ of 0.3Eu material
Ex=464nm) and excitation spectrum (λ
Em=611nm).
Fig. 7 is Sr among the embodiment
2La
0.7TaO
6: the emission spectrum (λ of 0.3Eu material
Ex=394nm) and excitation spectrum (λ
Em=613nm).
Fig. 8 is Ba among the embodiment
2La
0.7TaO
6: the emission spectrum (λ of 0.3Eu material
Ex=283nm) and excitation spectrum (λ
Em=594nm).
Fig. 9 is Ba among the embodiment
2Y
0.7TaO
6: the emission spectrum (λ of 0.3Eu material
Ex=266nm) and excitation spectrum (λ
Em=595nm).
Embodiment
Mode with embodiment illustrates the present invention below, but the present invention only limits to embodiment absolutely not.
Embodiment 1
With raw materials of Ca CO
3, Eu
2O
3, Nb
2O
5According to Ca
2EuNbO
6Stoichiometric ratio carry out weighing, after in mortar, mixing, in the corundum crucible with cover of packing in 625 ℃ of pre-burning 24h.After fully grinding, the gained powder fires 24h respectively in 1000 ℃, 1200 ℃, 1500 ℃ again.Make pure Ca
2EuNbO
6Fluorescent material.Test result is seen Fig. 1.
Embodiment 2
With raw materials of Ca CO
3, Eu
2O
3, Nb
2O
5According to Ca
2EuNbO
6Stoichiometric ratio carry out weighing, after in mortar, mixing, in the corundum crucible with cover of packing in the nitrogen atmosphere stove 625 ℃ of pre-burning 24h.After fully grinding, the gained powder fires 24h respectively in 1700 ℃ again.Make pure Ca2EuNbO6 fluorescent material.Test result is suitable with embodiment 1.
Embodiment 3
With raw materials of Ca CO
3, Eu
2O
3, Nb
2O
5According to Ca
2EuNbO
6Stoichiometric ratio carry out weighing, after in mortar, mixing, in the corundum crucible with cover of packing in the oxygen atmosphere stove 625 ℃ of pre-burning 24h.After fully grinding, the gained powder fires 24h respectively in 1300 ℃ again.Make pure Ca
2EuNbO
6Fluorescent material.Test result is suitable with embodiment 1.
Embodiment 4
With raw material SrCO
3, Eu
2O
3, Ta
2O
5According to Sr
2EuTaO
6Stoichiometric ratio carry out weighing, after in mortar, mixing, in the corundum crucible with cover of packing in 625 ℃ of pre-burning 24h.After fully grinding, the gained powder fires 24h respectively in 1000 ℃, 1200 ℃, 1500 ℃ again.Make pure Sr
2EuTaO
6Fluorescent material.It excites down at shortwave ultraviolet (250-350nm), near ultraviolet (393-395nm), blue light (463-465nm), effectively red-emitting (575-650nm).
With raw material SrCO
3, Eu
2O
3, Ta
2O
5According to according to Sr
0.2Ba
1.8EuTaO
6Stoichiometric ratio carry out weighing, after in mortar, mixing, in the corundum crucible with cover of packing in 625 ℃ of pre-burning 24h.After fully grinding, the gained powder fires 24h respectively in 1700 ℃ again.Make pure Sr0.2Ba1.8EuTaO6 fluorescent material.It excites down at shortwave ultraviolet (250-350nm), near ultraviolet (393-395nm), blue light (463-465nm), effectively red-emitting (575-650nm).
Embodiment 6
With raw material BaCO
3, Eu
2O
3, Ta
2O
5According to Ba
2EuTaO
6Stoichiometric ratio carry out weighing, after in mortar, mixing, in the corundum crucible with cover of packing in 625 ℃ of pre-burning 24h.After fully grinding, the gained powder fires 24h respectively in 1000 ℃, 1200 ℃, 1500 ℃ again.Make pure Ba
2EuTaO
6Fluorescent material.It excites down at shortwave ultraviolet (250-350nm), near ultraviolet (393-395nm), blue light (463-465nm), effectively red-emitting (575-650nm).
Embodiment 7
With raw materials of Ca (NO
3)
24H
2O, Y
2O
3, Nb
2O
5According to Ca
2YNbO
6Stoichiometric ratio carry out weighing, after in mortar, mixing, in the corundum crucible with cover of packing in 625 ℃ of pre-burning 24h.After fully grinding, the gained powder fires 24h respectively in 1000 ℃, 1200 ℃, 1500 ℃ again.Make pure Ca
2YNbO
6With gained Ca
2YNbO
6Powder and MnO press Ca
2YNbO
6: the proportioning of xMn (x=0.2) is ground evenly, places the sealing by fusing silica tube that vacuumizes to carry out follow-up doping in 950 ℃ of reaction 24h then.Obtain Ca
2YNbO
6: the Mn fluorescent material.It shows red broadband emission (550-700nm) under short wave ultraviolet excitation.
Embodiment 8
With raw materials of Ca CO
3, La (NO
3)
36H
2O, Ta
2O
5According to Ca
2LaTaO
6Stoichiometric ratio carry out weighing, after in mortar, mixing, in the corundum crucible with cover of packing in 625 ℃ of pre-burning 24h.After fully grinding, the gained powder fires 24h respectively in 1000 ℃, 1200 ℃, 1400 ℃ again.Make pure Ca
2LaTaO
6With gained Ca
2LaTaO
6Powder and MnO press Ca
2LaTaO
6: the proportioning of xMn (x=0.3) is ground evenly, places the sealing by fusing silica tube that vacuumizes to carry out follow-up doping in 950 ℃ of reaction 24h then.Obtain Ca
2LaTaO
6: the Mn fluorescent material.It shows red broadband emission (550-700nm) under short wave ultraviolet excitation.
Embodiment 9
With raw materials of Ca (CH
3COO)
2H
2O, Gd
2O
3, Nb
2O
5, according to Ca
2GdNbO
6Stoichiometric ratio carry out weighing, after mixing in mortar, the corundum crucible with cover of packing into is in 625 ℃ of pre-burning 24h.After fully grinding, the gained powder fires 24h respectively in 1150 ℃, 1200 ℃, 1400 ℃ again.Make unadulterated Ca
2GdNbO
6The fluorescent material body material.With gained Ca
2GdNbO
6Powder and Bi
2O
3Press Ca
2GdNbO
6: the proportioning of xBi (x=0.3) is ground evenly, places the sealing by fusing silica tube that vacuumizes to carry out follow-up doping in 930 ℃ of reaction 30h then.Obtain Ca
2GdNbO
6: the Bi fluorescent material.It shows strong blue light broadband emission under burst of ultraviolel.
With raw materials of Ca CO
3, La
2O
3, Y
2O
3, Ta
2O
5According to Ca
2La
0.9Y
0.1TaO
6Stoichiometric ratio carry out weighing, after mixing in mortar, the corundum crucible with cover of packing into is in 700 ℃ of pre-burning 20h.After fully grinding, the gained powder fires 24h respectively in 1100 ℃, 1250 ℃, 1400 ℃ again.Make unadulterated Ca
2La
0.9Y0
.1TaO
6The fluorescent material body material.With gained Ca
2La
0.9Y
0.1TaO
6Powder and Bi
2O
3Press Ca
2La
0.9Y0
.1Ta
O6: the proportioning of xBi (x=0.1) is ground evenly, places the sealing by fusing silica tube that vacuumizes to carry out follow-up doping in 950 ℃ of reaction 30h then.Obtain Ca
2La
0.9Y
0.1TaO
6: the Bi fluorescent material.It shows strong blue light broadband emission under burst of ultraviolel.
Embodiment 11
With raw materials of Ca CO
3, La
2O
3, Ta
2O
5According to Ca
2LaTaO
6Stoichiometric ratio carry out weighing, after mixing in mortar, the corundum crucible with cover of packing into is in 700 ℃ of pre-burning 20h.After fully grinding, the gained powder fires 24h respectively in 1100 ℃, 1250 ℃, 1400 ℃ again.Make unadulterated Ca
2LaTaO
6The fluorescent material body material.With gained Ca
2LaTaO
6Powder and Bi
2O
3Press Ca
2LaTaO
6: the proportioning of xBi (x=0.1) is ground evenly, places the sealing by fusing silica tube that vacuumizes to carry out follow-up doping in 950 ℃ of reaction 30h then.Obtain Ca
2LaTaO
6: the Bi fluorescent material.It shows strong blue light broadband emission under burst of ultraviolel.
Embodiment 12
With raw materials of Ca CO
3, Y (NO
3)
36H
2O, Nb
2O
5, Eu
2O
3According to Ca
2Y
1-xNbO
6: the stoichiometric ratio of xEu (x=0.05,0.3,0.75) is carried out weighing, and after mixing in mortar, the corundum crucible with cover of packing into is in 750 ℃ of pre-burning 12h.After fully grinding, the gained powder fires 24h respectively in 1100 ℃, 1250 ℃, 1500 ℃ again.Make Ca
2YNbO
6: the Eu fluorescent material.Test result is seen Fig. 2.
Embodiment 13
With raw materials of Ca CO
3, La (NO
3)
36H
2O, Nb
2O
5, Eu
2O
3According to Ca
2La
1-xNb0
6: the stoichiometric ratio of xEu (x=0.05,0.4,0.75) is carried out weighing, and after mixing in mortar, the corundum crucible with cover of packing into is in 750 ℃ of pre-burning 12h.After fully grinding, the gained powder fires 24h respectively in 1100 ℃, 1250 ℃, 1500 ℃ again.Make Ca
2LaNbO
6: the Eu fluorescent material.Test result is seen Fig. 3.
Embodiment 14
With raw materials of Ca CO
3, Gd
2O
3, Nb
2O
5, Eu
2O
3According to Ca
2Gd
1-xNbO
6: the stoichiometric ratio of xEu (x=0.05,0.5,0.75) is carried out weighing, and after mixing in mortar, the corundum crucible with cover of packing into is in 680 ℃ of pre-burning 20h.After fully grinding, the gained powder fires 24h, 24h, 48h respectively in 1100 ℃, 1250 ℃, 1450 ℃ again.Make Ca
2GdNbO
6: the Eu fluorescent material.Test result is seen Fig. 4.
With raw materials of Ca CO
3, Y
2O
3, Ta
2O
5, Eu
2O
3According to Ca
2Y
1-xTaO
6: the stoichiometric ratio of xEu (x=0.3) is carried out weighing, and after mixing in mortar, the corundum crucible with cover of packing into is in 680 ℃ of pre-burning 20h.After fully grinding, the gained powder fires 24h, 24h, 48h respectively in 1100 ℃, 1250 ℃, 1450 ℃ again.Make Ca
2YTaO
6: the Eu fluorescent material.Test result is seen Fig. 5.
Embodiment 16
With raw materials of Ca CO
3, Gd
2O
3, Ta
2O
5, Eu
2O
3According to Ca
2Gd
1-xTaO
6: (stoichiometric ratio of x=0.3 is carried out weighing to xEu, and after mixing in mortar, the corundum crucible with cover of packing into is in 700 ℃ of pre-burning 20h.After fully grinding, the gained powder fires 24h, 24h, 48h respectively in 1100 ℃, 1250 ℃, 1450 ℃ again.Make Ca
2GdTaO
6: the Eu fluorescent material.Test result is seen Fig. 5.
Embodiment 17
With raw materials of Ca CO
3, La
2O
3, Ta
2O
5, Eu
2O
3According to Ca
2La
1-xTaO
6: the stoichiometric ratio of xEu (x=0.3) is carried out weighing, and after mixing in mortar, the corundum crucible with cover of packing into is in 750 ℃ of pre-burning 20h.After fully grinding, the gained powder fires 24h, 24h, 48h respectively in 1100 ℃, 1250 ℃, 1450 ℃ again.Make Ca
2LaTaO
6: the Eu fluorescent material.Test result is seen Fig. 5.
Embodiment 18
With raw material SrCO
3, Gd
2O
3, Ta
2O
5, Eu
2O
3According to Sr
2Gd
1-xTaO
6.:xEu the stoichiometric ratio of (x=0.3) is carried out weighing, and after mixing in mortar, the corundum crucible with cover of packing into is in 650 ℃ of pre-burning 20h.After fully grinding, the gained powder fires 24h respectively in 1100 ℃, 1250 ℃, 1450 ℃ again.Make Sr
2GdTaO
6: the Eu fluorescent material.Test result is seen Fig. 6.
Embodiment 19
With raw material SrCO
3, La
2O
3, Ta
2O
5, Eu
2O
3According to Sr
2La
1-xTaO
6: the stoichiometric ratio of xEu (x=0.3) is carried out weighing, and after mixing in mortar, the corundum crucible with cover of packing into is in 650 ℃ of pre-burning 20h.After fully grinding, the gained powder fires 24h respectively in 1100 ℃, 1200 ℃, 1400 ℃ again.Make Sr
2LaTaO
6: the Eu fluorescent material.Test result is seen Fig. 7.
With raw material BaCO
3, La
2O
3, Ta
2O
5, Eu
2O
3According to Ba
2La
1-xTaO
6: the stoichiometric ratio of xEu (x=0.3) is carried out weighing, and after mixing in mortar, the corundum crucible with cover of packing into is in 650 ℃ of pre-burning 20h.After fully grinding, the gained powder fires 24h respectively in 1100 ℃, 1250 ℃, 1450 ℃ again.Make Ba
2LaTaO
6: the Eu fluorescent material.Test result is seen Fig. 8.
Embodiment 21
With raw material BaCO
3, Y (NO
3)
36H
2O, Ta
2O
5, Eu
2O
3According to Ba
2Y
1-xTaO
6: the stoichiometric ratio of xEu (x=0.3) is carried out weighing, and after mixing in mortar, the corundum crucible with cover of packing into is in 650 ℃ of pre-burning 20h.After fully grinding, the gained powder fires 24h respectively in 1100 ℃, 1200 ℃, 1400 ℃ again.Make Ba
2YTaO
6: the Eu fluorescent material.Test result is seen Fig. 9.
Embodiment 22
With raw materials of Ca CO
3, La
2O
3, Nb
2O
5, Eu
2O
3, Bi
2O
3According to Ca
2LaNbO
6: Bi
y, Eu
z(y=0.01, stoichiometric ratio z=0.3) is carried out weighing, and after mixing in mortar, the corundum crucible with cover of packing into is in the following 650 ℃ of pre-burning 20h of Ar atmosphere.After fully grinding, the gained powder fires 24h, 24h, 48h respectively in 1100 ℃, 1250 ℃, 1500 ℃ again.Make Ca
2LaNbO
6: Bi, Eu fluorescent material.It shows the biobelt emission of blue light and ruddiness under burst of ultraviolel.
Embodiment 23
With raw material Gd
2O
3, Nb
2O
5, Eu
2O
3According to Gd
1-xNbO
4: the stoichiometric ratio of xEu (x=0.3) is carried out weighing, and after mixing in mortar, the corundum crucible with cover of packing into is in the following 650 ℃ of pre-burning 20h of nitrogen atmosphere.After fully grinding, the gained powder fires 24h respectively in 1100 ℃, 1200 ℃, 1500 ℃ again.Make GdNbO
4: the Eu fluorescent material.It shows red emission under burst of ultraviolel.
Claims (10)
1. be used for niobate or the tantalite fluorescent material of white light LEDs, it is characterized in that chemical formula is A
aM
bM '
cO
d: M
II x, wherein:
A is one or more in second main group element;
M is one or more in the 3rd main group element or Sc or Y or the lanthanide series rare-earth elements;
M ' is a kind of among Nb or the Ta;
M
IIBe to be selected to have s
2In the class Tl ion of configuration one or more;
0＜a≤2，0＜b≤3，0＜c≤3，0＜d≤14，0＜x≤0.5。
2. by claim 1 described niobate or tantalite fluorescent material for white light LEDs, it is characterized in that, wherein:
A is one or more among Ca, Sr or the Ba;
M is one or more among Al, Ga, In, Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb or the Lu.
3. by claim 1 described niobate or tantalite fluorescent material for white light LEDs, it is characterized in that, wherein:
M
IIBe among Bi, Sb, Pb or the Sn one or more.
4. by claim 1 described niobate or tantalite fluorescent material for white light LEDs, it is characterized in that material possesses arbitrary structures, comprise perovskite structure, counterfeit perovskite structure, structure of double perovskite, olivine structural or pyrochlore structure.
5. by claim 4 described niobate or tantalite fluorescent material for white light LEDs, it is characterized in that material possesses counterfeit perovskite structure, structure of double perovskite or pyrochlore structure.
6. by claim 5 described niobate or tantalite fluorescent material for white light LEDs, it is characterized in that material possesses structure of double perovskite.
7. be used for the niobate of white light LEDs or the preparation method of tantalite fluorescent material, it is characterized in that, comprise the steps:
Step (1): press chemical formula
A
aM
bM '
cO
d: M
IIJoin and get raw material, wherein:
A is one or more in second main group element, one or more among preferred Ca, Sr or the Ba;
M is one or more in the 3rd main group element or Sc or Y or the lanthanide series rare-earth elements, one or more among preferred Al, Ga, In, Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb or the Lu;
M ' is a kind of among Nb or the Ta;
M
IIBe to be selected to have s
2In the class Tl ion of configuration one or more, one or more among preferred Bi, Sb, Pb or the Sn;
0＜a≤2，0＜b≤3，0＜c≤3，0＜d≤14，0＜x≤5。
Described raw material is the inorganic salt of each element;
Step (2): with 500～750 ℃ of pre-burnings under vacuum, air, oxygen, rare gas element or reducing gas environment of above-mentioned whole raw materials, the preferred reaction times is 0.1～48 hour.
Step (3): with 1000～1700 ℃ of high-temperature calcinations under vacuum, air, oxygen, rare gas element or reducing gas environment of step (2) products therefrom, the preferred reaction times is 12～72 hours.
8. by the preparation method of described niobate or the tantalite fluorescent material for white light LEDs of claim 7, it is characterized in that, behind completing steps (2), to step (2) products therefrom repeating step (2) repeatedly.
9. by the preparation method of described niobate or the tantalite fluorescent material for white light LEDs of claim 7, it is characterized in that, behind completing steps (3), to step (3) products therefrom repeating step (3) repeatedly.
10. by the preparation method of described niobate or the tantalite fluorescent material for white light LEDs of claim 7, it is characterized in that, behind completing steps (3), step (3) products therefrom is heat-treated under the reducing gas environment.
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Application publication date: 20130717 |