CN109722245A - Carbonitride phosphor powder containing lutetium, preparation method and the device containing the fluorescent powder - Google Patents
Carbonitride phosphor powder containing lutetium, preparation method and the device containing the fluorescent powder Download PDFInfo
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- CN109722245A CN109722245A CN201811069084.9A CN201811069084A CN109722245A CN 109722245 A CN109722245 A CN 109722245A CN 201811069084 A CN201811069084 A CN 201811069084A CN 109722245 A CN109722245 A CN 109722245A
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Abstract
The invention belongs to luminescent material technical fields, and in particular to a kind of lutetium base carbonitride phosphor powder, preparation method and the device containing the fluorescent powder.Fluorescent powder provided by the present invention includes that general formula is following inorganic compound: M1 2‑a‑xLuaM2 bM3 cNdCe: xCe, wherein M1Element is selected from one or both of Y, La, Gd rare earth cation；M2Selected from one or both of quadrivalent elements such as Si, Ge；M3Selected from one or both of Al, Ga, B triad；1≤a < 2,3.0 <b < 4.0,0 < c≤1,6.0 < d < 7.0,0 < e < 1,0.005≤x≤0.3, a+x≤2.Fluorescent powder of the invention have the characteristics that efficiently, uniformly, without miscellaneous phase, and preparation method is simple, is easy to industrialize.Its outstanding advantages is: compared with current technology, there is higher thermal quenching performance, it is photochromic in larger range tunable.The white light LEDs that this fluorescent powder is excited especially suitable for UV-Purple.
Description
Technical field
The invention belongs to luminescent material technical fields, and in particular to a kind of lutetium base carbonitride phosphor powder, preparation method
And the device containing the fluorescent powder.
Background technique
Compared with conventional light emitting device, light emitting diode (LED) is used as a kind of new and effective light source, the low, light with voltage
The advantages that effect is high, low energy consumption, the service life is long, pollution-free, at the same have small in size, response is fast, fever less and the spies such as reliability height
Point becomes the strategic new industry that 21 century China gives priority to.The especially development of white light source (being suitable for general illumination)
It plays a very important role for electric consumption on lighting measurer is greatly lowered.
Currently, realizing that the main path of white light LEDs is with blue light (440-470nm) LED chip excitated fluorescent powder complex group
At white light.There are two types of common combination sides: first, blue-light LED chip and yellow fluorescent powder combination；Secondly being blue-light LED chip
It is combined with red, green emitting phosphor.Wherein, garnet structure yellow fluorescent powder (YAG) matching blue-light LED chip because its efficiently,
It makes the advantages that simple and is widely used, but since spectrum poor continuity, red light portion lack, cause white light LED part
Colour rendering index is relatively low, colour temperature is higher, it is difficult to meet high-quality lighting demand.Therefore, on this basis by addition rouge and powder or
High color rendering index (CRI) white light is obtained by the way of red, green emitting phosphor using blue chip excitation.
In recent years, as the increasingly raising of people's living standard and semiconductor illumination technique are constantly progressive, people are to strong
Enhancing is realized in the concern of health and quality life, and the requirement to illumination has been increasingly turned to from simple environmental protection and energy saving comfortable to health
Pursuit.Tradition is composed White LED by blue LED die and other color fluorescence bodies, and it is unbalanced that there are emission wavelengths, green
The disadvantages of coloured light excalation, the peak strength for being particularly present blue light is higher, easily causes physiology, psychology of people etc.
The problem of, it is difficult to meet the needs of people are to health.Therefore, researcher propose to be applied in combination in purple LED chip red (R),
The White LED of green (G), blue (B) fluorophor.Compared with blue chip, this method purple light conversion of white light is more efficient, light
Spectral structure is balanced, and colour rendering index is relatively more preferable, but the chemistry and thermal stability etc. to fluorescent powder is put forward higher requirements, urgently
Suitable high density energy excitation to be developed, meet full spectrum high-quality illumination, suitable for purple or it is near ultraviolet excitated it is novel it is blue,
Green, red fluorescence powder.
Carbonitride is because of its stable physicochemical properties, the advantages that mild synthesis condition, and is ground by luminescent material
The extensive concern for the person of studying carefully.
RE2Si4N6C (RE=Y, Lu, Gd, La etc.) is by MRESi4N7(M=Ca, Sr, Ba；RE=Yb, Y) (referred to as 1147) drill
Become, by trivalent RE3+Replace divalent M2+, in order to make up charge balance, the [N (N in 11473)4] by [C (N3)4] replace, i.e.,
Obtain RE2Si4N6C.The RE of different rare earth ions doping2Si4N6C (RE=Y, Lu, Gd) has preferable luminescent properties, such as CN
Disclosed in 1922285 A, US 8007683B2,102585822 A of CN etc..In Lu2Si4N6In C, there are two types of coordinations by Lu, divide
It is not pentacoordinate and hexa-coordinate, activator Ce3+It is preferential to replace hexa-coordinate Lu3+, excitation spectrum covering 300-475nm, transmitting light
Spectrum peak wavelength be located at 540nm (Duan C, Zhang Z,S,et al.Preparation,
Characterization,and Photoluminescence Properties of Tb3+,Ce3+,and Ce3+/Tb3+-
Activated RE2Si4N6C (RE=Lu, Y, and Gd) Phosphors [J] .Chemistry of Materials, 2011,
23(7):1851-1861.).But in existing literature is reported, Lu2Si4N6C:Ce3+Emission spectrum it is single, photochromic tuning
Property is poor, and stability is poor.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of carbonitride phosphor powder containing lutetium, the fluorescent powder is suitable
The green emitting phosphor wide for the wide half-wave of near ultraviolet-purple excitation, photochromic tunable, hot-quenching, which is gone out, to have good stability.
The present invention also provides the preparation methods of above-mentioned fluorescent powder；
And the luminescent device containing above-mentioned fluorescent powder.
Carbonitride phosphor powder containing lutetium of the invention is the technical problem more than being solved by following technical solutions:
A kind of carbonitride phosphor powder containing lutetium is following inorganic compound: M comprising general formula1 2-a-xLuaM2 bM3 cNdCe:
XCe, wherein M1Element is selected from the combination of one or more of Y, La, Gd rare earth cation；M2Selected from Si, Ge
One or both of quadrivalent element；M3Combination selected from one or more of Al, Ga, B triad；And 1≤a <
2,3.0 <b < 4.0,0 < c≤1,6.0 < d < 7.0,0 < e < 1,0.005≤x≤0.3, a+x≤2.
Preferably, a+x < 2,0 < c≤1, b+c=4,6 < d < 7.0,0 < e < 1,0.05≤x≤0.2.
M1For La and/or Y element；
Preferably, M2Selected from Si element；
M3Selected from Al element；
M1It is preferred that La and/or Y element, M2Selected from Si element, M3Selected from Al element.
Between 300-450nm, the peak wavelength of emission spectrum is located at the peak wavelength of the excitation spectrum of fluorescent powder
Between 480-520nm.
A+x=2,0 < c≤1, b+c=4,6.0 < d < 7.0,0 < e < 1,0.05≤x≤0.2.
M2Selected from Si element；
Preferably, M3Selected from Al element；
Preferably, M2Selected from Si element, M3Selected from Al element.
For the peak wavelength of fluorescent powder excitation spectrum between 300-450nm, the peak wavelength of emission spectrum is located at 530-
Between 570nm.
The method for preparing the above-mentioned carbonitride phosphor powder containing lutetium, includes the following steps:
(1) by M1、M2、M3, simple substance or compound and carbon source corresponding to Lu and Ce stoichiometrically weigh, it is finely ground, mix
It is even, obtain mixture；
(2) by mixture high temperature sintering under protective atmosphere obtained by step (1), carbonitride phosphor powder containing lutetium is obtained.
Lu, M in step (1)1, compound corresponding to Ce be Lu, M1, Ce nitride, oxide, carbonate or nitrate
Middle a combination of one or more；M2、M3Corresponding compound is M2、M3Nitride, a kind of in carbide or oxide
Or two or more combination；
Preferably, carbon source is graphite, active carbon, amorphous carbon, sucrose, a combination of one or more in urea；
Preferably, protective atmosphere is Ar, N in step (2)2、Ar/H2Or N2/H2The group of middle one or more
It closes；
Preferably, high temperature sintering is once sintered or multiple sintering；
Preferably, the temperature of sintering is 1400-1900 DEG C, and the time of sintering is 2-20h.
Preferably, it is cooled to room temperature after sintering and is post-processed to obtain fluorescent powder；
Preferably, post-processing includes the process be crushed, grind, being classified, sieving and washing.
A kind of luminescent device prepares resulting fluorescent powder comprising light source and by above-mentioned method.
The beneficial effects of the present invention are fluorescent powder of the invention has wider excitation peak, is especially suitable for purple, near ultraviolet
Excitation has preferable applicability；
And the Emission Spectrum Peals wavelength of above-mentioned fluorescent powder 480-590nm have coordinability, and half-wave it is wide compared with
Greatly, the spectrum between blue green light to green-yellow light can be effectively covered, especially suitable for full spectral illumination.
Compared with prior art, there is fluorescent powder of the invention superior hot-quenching to go out performance.
Detailed description of the invention
Fig. 1 is the material phase analysis of comparative example and 1 gained fluorescent powder of embodiment；
Fig. 2 is the excitation spectrum of comparative example and 1 gained fluorescent powder of embodiment；
Fig. 3 is the emission spectrum of comparative example and 1 gained fluorescent powder of embodiment；
Fig. 4 is the thermal stability comparison of comparative example and embodiment 1；
Fig. 5 is the shape appearance figure of embodiment 2；
Fig. 6 is the launching light spectrogram for encapsulating white light LED part；
Fig. 7 is device pictorial diagram.
Specific embodiment
Next with reference to the accompanying drawings and detailed description the present invention will be further explained, so as to the technology of this field
Personnel know more about the present invention, but do not limit the present invention with this.
Comparative example
By the chemical formula (Lu of fluorescent powder0.98,Ce0.02)2Si4N6C weighs 3.509g Lu respectively2O3、1.683g Si3N4、
0.477g C、0.061g CeO2.After abundant mix grinding is uniform, mixture is placed in tungsten matter crucible, in N2It is roasted in atmosphere,
Sintering temperature is 1750 DEG C, and calcining time is 10 hours, with room temperature natural cooling.Product of roasting is crushed, be classified, is washed
The post-processing such as washing, dry and sieve becomes (Lu to get group0.98,Ce0.02)2Si4N6The fluorescent powder of C.
Fig. 1 is the material phase analysis figure that product is made in the comparative example.Material phase analysis itself and Ho as the result is shown2Si4N6The crystal of C
Structure is similar.
The comparative example be made product excitation spectrum (525nm monitoring) and emission spectrum (425nm excitation) respectively such as Fig. 2 with
Shown in Fig. 3, it can be seen that its excitation wavelength range covers 300~475nm, and launch wavelength covers 450~650nm, peak value wave
It is long to be located at 525nm.
Fig. 4 is relative intensity variation with temperature curve, and the emissive porwer of 150 DEG C of display is 65% at room temperature in figure.
Embodiment 1
By the chemical formula (Lu of fluorescent powder0.98,Ce0.02)2Si3.8Al0.2N6.2C0.8, 3.509g Lu is weighed respectively2O3、
1.599g Si3N4、0.074gAlN、0.477g C、0.061g CeO2.After abundant mix grinding is uniform, mixture is placed in tungsten matter earthenware
In crucible, in N2It is roasted in atmosphere, sintering temperature is 1750 DEG C, and calcining time is 10 hours, with room temperature natural cooling.It will roasting
It burns product and the post-processing such as is crushed, be classified, washed, dries and sieve to get group as (Lu0.98,Ce0.02)2Si3.8Al0.2N6.2C0.8Fluorescent powder.
Its material phase analysis shows that the crystal structure and Ho of product is made in the embodiment in Fig. 12Si4N6The crystal structure phase of C
Seemingly.In Fig. 1, abscissa is 2 θ, means that the X-ray diffraction spectrum is X-ray diffractometer with the entire diffraction region of the angle scanning of 2 θ,
As angle change, ordinate is that intrnsity is diffracted intensity；
Fig. 2 and Fig. 3 show that the excitation wavelength range that product is made in the embodiment of the present invention 1 covers 300~475nm, transmitting
Wavelength covers 450~650nm, and peak wavelength is located at 531nm, and red shift has occurred in peak wavelength compared with comparative example, realizes light
The tunability of color.
It is shown in Fig. 4,150 DEG C of emissive porwer is at room temperature 70%, is significantly improved compared with comparative example, i.e. its heat
It is quenching to significantly improve.(in Fig. 2 and Fig. 3, abscissa is wavelength, and ordinate is emissive porwer value)
Embodiment 2
By chemical formula Lu1.95Ce0.05Si3.4Al0.6N6.6C0.4Stoichiometric, accurately weigh LuN (purity
99.9%), Si3N4(purity 99.9%), AlN (purity 99.9%), SiC (purity 99.9%) and CeN (purity 99.99%) are former
Material, and it is mixed to form mixed raw material.Mixture is obtained after mixed raw material to be adequately mixed to grinding 30min in glove box.It will
Mixture is raised to 1700 DEG C with the heating rate of 10 DEG C/min, and then in 1700 DEG C of heat preservation 10h, Temperature fall obtains roasting and produces
Object.It after product of roasting is taken out, is crushed, washed, is sieved and dried, obtain embodiment 2
Lu1.95Ce0.05Si3.4Al0.6N6.6C0.4Fluorescent powder.The SEM pattern of embodiment 2 is as shown in Fig. 5.
Embodiment 3
By chemical formula Lu1.95Ce0.05Si3.9Al0.1N6.1C0.9Stoichiometric, accurately weigh LuH3(purity
99.9%), Si3N4(purity 99.9%), AlN (purity 99.9%), SiC (purity 99.9%) and CeN (purity 99.99%) are former
Material, and it is mixed to form mixed raw material.Mixture is obtained after mixed raw material to be adequately mixed to grinding 30min in glove box.It will
Mixture is raised to 1730 DEG C with the heating rate of 10 DEG C/min, and then in 1730 DEG C of heat preservation 10h, Temperature fall obtains roasting and produces
Object.It after product of roasting is taken out, is crushed, washed, is sieved and dried, obtain embodiment 3
Lu1.95Ce0.05Si3.9Al0.1N6.1C0.9Fluorescent powder.
Embodiment 4
By chemical formula Lu1.9Ce0.1Si3.5Al0.5N6.5C0.5Stoichiometric, accurately weigh Lu (purity 99.9%),
Si3N4(purity 99.9%), AlN (purity 99.9%), SiC (purity 99.9%) and CeN (purity 99.99%) raw material, and mix
Form mixed raw material.Mixture is obtained after mixed raw material to be adequately mixed to grinding 30min in glove box.By mixture with 10
DEG C/heating rate of min is raised to 1800 DEG C, then in 1800 DEG C of heat preservation 10h, Temperature fall obtains product of roasting.Roasting is produced
After object takes out, it is crushed, is washed, is sieved and is dried, obtain the Lu of embodiment 41.9Ce0.1Si3.5Al0.5N6.5C0.5Fluorescent powder.
Embodiment 5
By chemical formula Lu1.94Ce0.06Si3.95Al0.05N6.05C0.95Stoichiometric, accurately weigh Lu2(CO3)3It is (pure
It spends 99.9%), Al2O3(purity 99.9%), Si3N4(purity 99.9%), C (purity 99.9%) and CeN (purity 99.99%)
Raw material, and it is mixed to form mixed raw material.Mixture is obtained after mixed raw material to be adequately mixed to grinding 30min in glove box.
Mixture is raised to 1900 DEG C with the heating rate of 10 DEG C/min, then in 1900 DEG C of heat preservation 10h, Temperature fall obtains roasting and produces
Object.It after product of roasting is taken out, is crushed, washed, is sieved and dried, obtain embodiment 5
Lu1.94Ce0.06Si3.95Al0.05N6.05C0.95Fluorescent powder.
Embodiment 6
By chemical formula Lu1.5Y0.44Ce0.06Si3.6Al0.4N6.4C0.6Stoichiometric, accurately weigh YN (purity
99.9%), LuN (purity 99.9%), Si3N4(purity 99.9%), AlN (purity 99.9%), SiC (purity 99.9%) and CeN
(purity 99.99%) raw material, and it is mixed to form mixed raw material.Mixed raw material is adequately mixed to grinding 30min in glove box
After obtain mixture.Mixture is raised to 1700 DEG C with the heating rate of 10 DEG C/min, it is natural then in 1700 DEG C of heat preservation 10h
Cooling obtains product of roasting.It after product of roasting is taken out, is crushed, washed, is sieved and dried, obtain embodiment 6
Lu1.5Y0.44Ce0.06Si3.6Al0.4N6.4C0.6Fluorescent powder.
Embodiment 7
By chemical formula LuLa0.94Ce0.06Si3.95Al0.05N6.05C0.95Stoichiometric, accurately weigh LaN (purity
99.9%), LuN (purity 99.9%), Si3N4(purity 99.9%), AlN (purity 99.9%), SiC (purity 99.9%) and CeN
(purity 99.99%) raw material, and it is mixed to form mixed raw material.Mixed raw material is adequately mixed to grinding 30min in glove box
After obtain mixture.Mixture is raised to 1800 DEG C with the heating rate of 10 DEG C/min, it is natural then in 1800 DEG C of heat preservation 10h
Cooling obtains product of roasting.It after product of roasting is taken out, is crushed, washed, is sieved and dried, obtain embodiment 7
LuLa0.94Ce0.06Si3.95Al0.05N6.05C0.95Fluorescent powder.
Embodiment 8
By chemical formula LuGd0.94Ce0.06Si3.05Al0.95N6.95C0.05Stoichiometric, accurately weigh LuN (purity
99.9%), GdN (purity 99.9%), Si3N4(purity 99.9%), AlN (purity 99.9%), SiC (purity 99.9%) and CeN
(purity 99.99%) raw material, and it is mixed to form mixed raw material.Mixed raw material is adequately mixed to grinding 30min in glove box
After obtain mixture.Mixture is raised to 1780 DEG C with the heating rate of 10 DEG C/min, it is natural then in 1780 DEG C of heat preservation 10h
Cooling obtains product of roasting.It after product of roasting is taken out, is crushed, washed, is sieved and dried, obtain embodiment 8
LuGd0.94Ce0.06Si3.05Al0.95N6.95C0.05Fluorescent powder.
Embodiment 9
(the Lu that above-described embodiment 1 is obtained0.98,Ce0.02)2Si3.8Al0.2N6.2C0.8With blue emitting phophor BAM:Eu2+, it is red
Color fluorophor CaAlSiN3:Eu2+, the mass ratio of three kinds of fluorophor is to form sicker in 4:1:2 mixing addition silica gel, by gluing
Object is coated on 405nm near ultraviolet LED chip, obtains white light LED part, surveys light integral by distant place SIS-3_1.0m steel
Ball _ R98, driving current 60mA, detection obtain the colour rendering index of the white light LED part be 96.6, colour temperature 4159K.(attached drawing
6 be the launching light spectrogram of white light LED part, and as can be seen from Figure 6 blue green light partial spectrum solves background skill than more uniform
Tradition is composed its there are emission wavelengths unbalanced, cyan of White LED by blue LED die and other color fluorescence bodies in art
This defect such as light excalation, the higher attached drawing 7 of peak strength for being particularly present blue light is pictorial diagram).
The emission peak wavelength result of the fluorescent powder of the above various embodiments such as table 1.Colour rendering index is tested using HAAS2000.
The proportion composition of each raw material in 1 comparative example of table and embodiment
It need to be noted that be a, b, c, d, e, x respectively indicate different elements in the specific molecular formula of each embodiment sample
Corresponding stoichiometric ratio.
If can be seen that M according to above-mentioned test data1Using Lu as standard, when gradually being replaced by La, emission spectrum occurs blue
It moves；When gradually being replaced by Gd/Y, red shift gradually occurs for emission spectrum.Work as M2When the Si of case is gradually replaced by Al, emit light
Red shift gradually occurs for spectrum.
In addition, the X-ray ray scan of the fluorescent powder of above-described embodiment 1-7 shows have and Y2Si4N6C is similar
Diffraction maximum, structure refinement is carried out to it using Rietveld method, the results showed that all have and Y2Si4N6The identical crystal knot of C
Structure.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of carbonitride phosphor powder containing lutetium, which is characterized in that the fluorescent powder includes that general formula is following inorganic compound:
M1 2-a-xLuaM2 bM3 cNdCe: xCe, wherein M1Element is selected from one or more of Y, La, Gd rare earth cation
Combination；M2Selected from one or both of Si, Ge quadrivalent element；M3Selected from one or more of Al, Ga, B triad
Combination；And 1≤a < 2,3.0 <b < 4.0,0 < c≤1,6.0 < d < 7.0,0 < e < 1,0.005≤x≤0.3, a+x≤2.
2. carbonitride phosphor powder containing lutetium according to claim 1, which is characterized in that a+x < 2,0 < c≤1, b+c=4,6 <
D < 7.0,0 < e < 1,0.05≤x≤0.2.
3. carbonitride phosphor powder containing lutetium according to claim 1 or 2, which is characterized in that M1Preferably La and/or Y member
Element；Either M2Preferably Si element；Either M3Preferably Al element；
It is either preferred, M1For La and/or Y element, M2For Si element；
It is either preferred, M2For Si element, M3For Al element；
It is either preferred, M1For La and/or Y element, M3For Al element；
It is either preferred, M1For La and/or Y element, M2For Si element, M3For Al element.
4. carbonitride phosphor powder containing lutetium according to any one of claim 1-3, which is characterized in that the excitation of fluorescent powder
The peak wavelength of spectrum is between 300-450nm, and the peak wavelength of emission spectrum is between 480-520nm.
5. carbonitride phosphor powder containing lutetium according to claim 1, which is characterized in that a+x=2,0 < c≤1, b+c=4,
6.0 < d < 7.0,0 < e < 1,0.05≤x≤0.2.
6. carbonitride phosphor powder containing lutetium according to claim 5, which is characterized in that M2Preferably Si element；Either M3
Preferably Al element；
It is either preferred, M2For Si element, M3For Al element.
7. the carbonitride phosphor powder containing lutetium according to any one of claim 5-6, which is characterized in that fluorescent powder exciting light
The peak wavelength of spectrum is between 300-450nm, and the peak wavelength of emission spectrum is between 530-570nm.
8. the method for preparing the carbonitride phosphor powder containing lutetium described in claim 1, includes the following steps:
(1) by M1、M2、M3, simple substance or compound and carbon source corresponding to Lu and Ce stoichiometrically weigh, it is finely ground, mix,
Obtain mixture；
(2) by mixture high temperature sintering under protective atmosphere obtained by step (1), carbonitride phosphor powder containing lutetium is obtained.
Preferably, Lu, M in step (1)1, compound corresponding to Ce be Lu, M1, Ce nitride, oxide, carbonate or nitric acid
At least one of in salt；
Preferably, M2、M3Corresponding compound is M2、M3At least one of nitride, carbide or oxide；
Preferably, carbon source is at least one of graphite, active carbon, amorphous carbon, sucrose, urea；
Preferably, protective atmosphere is Ar, N in step (2)2、Ar/H2Or N2/H2Middle a combination of one or more；
Preferably, high temperature sintering is once sintered or multiple sintering；
Preferably, the temperature of sintering is 1400-1900 DEG C, and the time of sintering is 2-20h；
Preferably, it is cooled to room temperature after sintering and is post-processed to obtain fluorescent powder；
Preferably, post-processing includes the process be crushed, grind, being classified, sieving and washing.
9. application of the fluorescent powder in luminescent device described in any one of claim 1-7, or pass through claim 8
In method preparation application of the fluorescent powder in luminescent device.
10. a kind of luminescent device includes light source and fluorescent powder, it is characterised in that: the fluorescent powder includes to appoint in claim 1-7
Fluorescent powder described in one；Either the fluorescent powder includes the fluorescent powder that method for claim 8 prepares.
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| CN109722245B (en) | 2022-05-10 |
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Address after: 100088, 2, Xinjie street, Xicheng District, Beijing Patentee after: GRIREM ADVANCED MATERIALS Co.,Ltd. Patentee after: Youyan rare earth high technology Co., Ltd Address before: 100088, 2, Xinjie street, Xicheng District, Beijing Patentee before: GRIREM ADVANCED MATERIALS Co.,Ltd. Patentee before: Guoke rare earth new material Co., Ltd |