CN109880622A - A method of light-emitting phosphor intensity is enhanced based on nitridation - Google Patents
A method of light-emitting phosphor intensity is enhanced based on nitridation Download PDFInfo
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- CN109880622A CN109880622A CN201910202420.0A CN201910202420A CN109880622A CN 109880622 A CN109880622 A CN 109880622A CN 201910202420 A CN201910202420 A CN 201910202420A CN 109880622 A CN109880622 A CN 109880622A
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- nitridation
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Abstract
The present invention relates to a kind of methods based on nitridation enhancing light-emitting phosphor intensity, realize luminescence enhancement by introducing nitrogen partial substitution of oxygen element, and with strontium aluminate (Sr4Al14O25) it is used as luminescent ceramic matrix, Eu2+As luminescent activator, HBO3As cosolvent, AlN enhancing is mixed in matrix and is shone, and blue-green fluorescent powder Sr is synthesized using high temperature solid-state method3.96Eu0.04Al14‑xAlxO25‑ xNx: xAlN, wherein 0%≤x≤25%.The present invention replaces oxygen element by the introducing portion of nitrogen, and the luminescent properties of fluorescent powder obtain at least 1.3 times or more of promotion;The present invention continues to use original preparation process, only need to increase a raw material on the original basis, and do not change original spectral signature, the fluorescent material easy to spread to other matrix.
Description
Technical field
The present invention relates to luminescent material technical field, especially a kind of side based on nitridation enhancing light-emitting phosphor intensity
Method.
Background technique
In recent years, since white light LEDs are due to its friendly, low energy consumption and high luminous efficiency to environment
The great research interest of people is caused with long fluorescence lifetime.White light LEDs (WLED) have energy-efficient, compact durable etc. excellent
Gesture, the universal of it will significantly reduce energy consumption.Fluorescent conversion type WLED (pc-WLED) is the most important implementation of current WLED,
The core material of this technology is fluorescent powder, directly determines the luminescent properties of final white light LED part.
So far, that realizes white light is broadly divided into following two approach, the first typical commercial white light LEDs, main
If passing through visible optical chip and YAG:Ce3+Yellow fluorescent powder combination;Second is smeared using three kinds of fluorescent powders of red, green, blue
In the method for UV-LED chip, this is a kind of warm white fluorescent powder tool that non-length effectively generates warm white approach, and obtains
There are higher colour rendering index (Ra > 80) and low color stability.The white fluorescent powder reported at present there is many problems, than
Such as poor chemical stability, low fluorescence efficiency, harsher synthesis condition etc..
As LED chip develops to shortwave direction (360nm-410nm), research and development can be by near ultraviolet excitated high-efficiency fluorescence powder
It will be significant.In addition to considering excitation wavelength factor, luminous intensity is also the important indicator of fluorescent powder, if can further be promoted
Luminous intensity then can more preferably play energy-conserving action.Usual luminous intensity can by changing doping concentration, introducing sensitizer ion,
Enhance activator ion luminous intensity by energy transmission or improve the modes such as appearance structure and gets a promotion.
Panchromatic white emitting fluorescent powder matrix used in field of LED illumination includes phosphate, aluminate, silicate, nitrogen at present
Silicon compound, sulfide etc.;It is slightly poor and aobvious that the chemical and thermal stability of aluminates system fluorescent powder compares other system fluorescent powders
Colour index is lower;SiO in silicate and halogen silicate matrix2Inertia causes more by force material phase structure complexity not easy to control;Nitrogen
The preparation condition of silicon compound is very harsh, it is desirable that sintering temperature is up to 2000 DEG C;Nitride and nitrogen oxides system fluorescent powder
Cost of material height and complex process, are not suitable for large-scale industrial production;Sulfide substrate fluorescent powder since light emission luminance is low and
It is greatly limited with harmful substance, therefore in practical applications.Therefore, rare earth ion doped single-matrix silicic acid
Salt base fluorescent powder is considered as a kind of up-and-coming luminescent material.Zhang Jiahua etc. is panchromatic single white using high temperature solid-state method preparation
Light BaMg2A16Si9O30: Eu2+, Tb2+, Mn2+Fluorescent powder, in this system, white light by 450nm, 540nm, 610nm 3 bands of a spectrum
Composition realizes photochromic best match, and (such as Zhang Jiahua, Lv Wei, Hao Zhendong are realized adjustable panchromatic single white using energy transmission
Light BaMg2Al6Si9O30: Eu2+, Tb3+, Mn2+Fluorescent powder (specially inviting) [J] Chinese Optical, 2012,5 (3): 203-208.).Ning Qing
Chrysanthemum, the patented technology " a kind of white light LEDs panchromatic fluorescent powder and preparation method thereof " of Qiao Changjun et al., using colloidal sol burning legal system
For Sr2-xMgSi2O7:xTb3+, the panchromatic phosphor for white light LED of single-matrix has been obtained, (China,
CN201310027088.1), therefore seek the research that the completely new rear-earth-doped single-matrix fluorescent powder of one kind is white light LEDs field
Emphasis.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of method based on nitridation enhancing light-emitting phosphor intensity, should
Method is not only at low cost, but also easy to spread.
The technical solution of the present invention is as follows: a kind of method based on nitridation enhancing light-emitting phosphor intensity, by introducing nitrogen member
Plain partial substitution of oxygen element realizes luminescence enhancement, and with strontium aluminate (Sr4Al14O25) it is used as luminescent ceramic matrix, Eu2+As
Luminescent activator, HBO3As cosolvent, AlN enhancing is mixed in matrix and is shone, and blue-green is synthesized using high temperature solid-state method
Fluorescent powder Sr3.96Eu0.04Al14-xAlxO25-xNx: xAlN, wherein 0%≤x≤25%.
Further, blue-green fluorescent powder Sr is synthesized using high temperature solid-state method3.96Eu0.04Al14-xAlxO25-xNx: xAlN tool
Body the following steps are included:
It S1), is Sr:Eu:Al:AlN=3.96:0.02:14-x:x according to molar ratio, wherein 0%≤x≤25%;Respectively
It weighs containing strontium, europium, aluminium compound raw material and aluminium nitride, and weighs the cosolvent HBO of gross mass 4%3;
S2), pre-burning in air atmosphere after being ground the raw material in step S1);
S3), the sample after the pre-burning in step S2) is taken out, in H after being ground2Or N2Mixing reducing atmosphere or carbon
Calcination under reducing atmosphere;
S4), the sample after calcination in step S3) is taken out, obtains blue-green fluorescent powder after being ground
Sr3.96Eu0.04Al14-xAlxO25-xNx: xAlN, wherein 0%≤x≤25%.
Further, step S1) in, the raw materials of compound containing strontium is strontium carbonate or strontium nitrate.
Further, step S1) in, the raw materials of compound containing europium is europiumsesquioxide.
Further, step S1) in, the raw materials of compound of the aluminium is aluminium hydroxide or aluminum oxide.
Further, step S1) in, the x=15%.
Further, step S2) in, calcined temperature is 700 DEG C, and soaking time is 2 hours.
Further, step S3) in, calcination temperature is 1400 DEG C, and soaking time is 5 hours.
The invention has the benefit that
1, oxygen element is replaced by the introducing portion of nitrogen, the luminescent properties of fluorescent powder prepared by the present invention obtain at least
1.3 times or more of promotion, such as Sr4Al14O25:Eu2+Luminescent properties improve 1.3 times or more;
2, the present invention continues to use original preparation process, only need to increase a raw material on the original basis, and do not change original
Spectral signature, the fluorescent material easy to spread to other matrix.
Detailed description of the invention
Fig. 1 is the X-ray diffraction spectrum figure of the fluorescent material of 1-6 of embodiment of the present invention preparation, and in figure, proportion one is to matching
Embodiment 1-6 is respectively corresponded than six.
Fig. 2 is the luminescent spectrum figure of the fluorescent material of 1-4 of embodiment of the present invention preparation, and in figure, proportion one to proportion four is divided
Other corresponding embodiment 1-4;
Fig. 3 is the relative luminous intensity figure of the fluorescent material of 1-6 of embodiment of the present invention preparation, wherein the value of x is respectively
0%, 5%, 10%, 15%, 20%, 25%, respectively correspond the x value in embodiment 1-6.
Specific embodiment
Specific embodiments of the present invention will be further explained with reference to the accompanying drawing:
Embodiment 1
A method of light-emitting phosphor intensity being enhanced based on nitridation, the present embodiment uses strontium aluminate (Sr4Al14O25) conduct
Luminescent ceramic matrix uses Eu2+As luminescent activator, HBO3As cosolvent, AlN enhancing is mixed in matrix and is shone, and is adopted
It is synthesized with high temperature solid-state method, specifically includes the following steps:
It S1), is Sr:Eu:Al:AlN=1.8082:0.0054:3.0399:0.0127 according to molar ratio, corresponding x=0%;
It weighs respectively and makees initial compounds containing strontium, europium, aluminium compound oxide spinel strontium, europiumsesquioxide, aluminium hydroxide and aluminium nitride
Raw material, and weigh the cosolvent HBO of gross mass 4%3;
S2), it is put into corundum crucible after being ground the raw material in step S1), then crucible is put into high-temperature electric resistance furnace
Pre-burning in air atmosphere, pre-burning 2h under conditions of temperature is 700 DEG C;
S3), the sample after the pre-burning in step S2) is taken out, crucible is put into after being ground, in H2And N2Mixing also
Under Primordial Qi atmosphere 1400 DEG C calcination 5 hours;
S4), the sample after calcination in step S3) is taken out, with furnace natural cooling, obtains blue-green fluorescent after being ground
Powder, X-ray diffraction analysis show it for Sr4Al14O25Phase.
Embodiment 2
A method of light-emitting phosphor intensity being enhanced based on nitridation, the present embodiment uses strontium aluminate (Sr4Al14O25) conduct
Luminescent ceramic matrix uses Eu2+As luminescent activator, HBO3As cosolvent, AlN enhancing is mixed in matrix and is shone, and is adopted
It is synthesized with high temperature solid-state method, specifically includes the following steps:
It S1), is Sr:Eu:Al:AlN=1.7512:0.0053:3.1077:0.0061 according to molar ratio, corresponding x=5%;
It weighs respectively and makees initial compounds containing strontium, europium, aluminium compound oxide spinel strontium, europiumsesquioxide, aluminium hydroxide and aluminium nitride
Raw material, and weigh the cosolvent HBO of gross mass 4%3;
S2), it is put into corundum crucible after being ground the raw material in step S1), then crucible is put into high-temperature electric resistance furnace
Pre-burning in air atmosphere, pre-burning 2h under conditions of temperature is 700 DEG C;
S3), the sample after the pre-burning in step S2) is taken out, crucible is put into after being ground, in 5% H2With 95%
N2Mixing reducing atmosphere under 1400 DEG C calcination 5 hours;
S4), the sample after calcination in step S3) is taken out, with furnace natural cooling, obtains blue-green fluorescent after being ground
Powder, X-ray diffraction analysis show it for Sr4Al14O25Phase.
Embodiment 3
A method of light-emitting phosphor intensity being enhanced based on nitridation, the present embodiment uses strontium aluminate (Sr4Al14O25) conduct
Luminescent ceramic matrix uses Eu2+As luminescent activator, HBO3As cosolvent, AlN enhancing is mixed in matrix and is shone, and is adopted
It is synthesized with high temperature solid-state method, specifically includes the following steps:
It S1), is Sr:Eu:Al:AlN=1.8082:0.0054:3.0399:0.0127 according to molar ratio, corresponding x=
10%;It weighs and is risen containing strontium, europium, aluminium compound oxide spinel strontium, europiumsesquioxide, aluminum oxide and aluminium nitride respectively
Beginning raw materials of compound, and weigh the cosolvent HBO of gross mass 4%3;
S2), it is put into corundum crucible after being ground the raw material in step S1), then crucible is put into high-temperature electric resistance furnace
Pre-burning in air atmosphere, pre-burning 2h under conditions of temperature is 700 DEG C;
S3), the sample after the pre-burning in step S2) is taken out, crucible is put into after being ground, in 5% H2With 95%
N2Mixing reducing atmosphere under 1400 DEG C calcination 5 hours;
S4), the sample after calcination in step S3) is taken out, with furnace natural cooling, obtains blue-green fluorescent after being ground
Powder, X-ray diffraction analysis show it for Sr4Al14O25Phase.
Embodiment 4
A method of light-emitting phosphor intensity being enhanced based on nitridation, the present embodiment uses strontium aluminate (Sr4Al14O25) conduct
Luminescent ceramic matrix uses Eu2+As luminescent activator, HBO3As cosolvent, AlN enhancing is mixed in matrix and is shone, and is adopted
It is synthesized with high temperature solid-state method, specifically includes the following steps:
It S1), is Sr:Eu:Al:AlN=1.8689:0.0056:2.9674:0.0197 according to molar ratio, corresponding x=
15%;It weighs and is risen containing strontium, europium, aluminium compound oxide spinel strontium, europiumsesquioxide, aluminum oxide and aluminium nitride respectively
Beginning raw materials of compound, and weigh the cosolvent HBO of gross mass 4%3;
S2), it is put into corundum crucible after being ground the raw material in step S1), then crucible is put into high-temperature electric resistance furnace
Pre-burning in air atmosphere, pre-burning 2h under conditions of temperature is 700 DEG C;
S3), the sample after the pre-burning in step S2) is taken out, crucible is put into after being ground, in 5% H2With 95%
N2Mixing reducing atmosphere under 1400 DEG C calcination 5 hours;
S4), the sample after calcination in step S3) is taken out, with furnace natural cooling, obtains blue-green fluorescent after being ground
Powder, X-ray diffraction analysis show it for Sr4Al14O25Phase.
Embodiment 5
A method of light-emitting phosphor intensity being enhanced based on nitridation, the present embodiment uses strontium aluminate (Sr4Al14O25) conduct
Luminescent ceramic matrix uses Eu2+As luminescent activator, HBO3As cosolvent, AlN enhancing is mixed in matrix and is shone, and is adopted
It is synthesized with high temperature solid-state method, specifically includes the following steps:
It S1), is Sr:Eu:Al:AlN=1.9339:0.0058:2.8900:0.0271 according to molar ratio, corresponding x=
20%;It weighs and is originated containing strontium, europium, aluminium compound oxide spinel strontium, europiumsesquioxide, aluminium hydroxide and aluminium nitride respectively
Raw materials of compound, and weigh the cosolvent HBO of gross mass 4%3;
S2), it is put into corundum crucible after being ground the raw material in step S1), then crucible is put into high-temperature electric resistance furnace
Pre-burning in air atmosphere, pre-burning 2h under conditions of temperature is 700 DEG C;
S3), the sample after the pre-burning in step S2) is taken out, crucible is put into after being ground, in 5% H2With 95%
N2Mixing reducing atmosphere under 1400 DEG C calcination 5 hours;
S4), the sample after calcination in step S3) is taken out, with furnace natural cooling, obtains blue-green fluorescent after being ground
Powder, X-ray diffraction analysis show it for Sr4Al14O25Phase.
Embodiment 6
A method of light-emitting phosphor intensity being enhanced based on nitridation, the present embodiment uses strontium aluminate (Sr4Al14O25) conduct
Luminescent ceramic matrix uses Eu2+As luminescent activator, HBO3As cosolvent, AlN enhancing is mixed in matrix and is shone, and is adopted
It is synthesized with high temperature solid-state method, specifically includes the following steps:
It S1), is Sr:Eu:Al:AlN=2.0035:0.0060:2.8070:0.0351 according to molar ratio, corresponding x=
25%;It weighs and is risen containing strontium, europium, aluminium compound oxide spinel strontium, europiumsesquioxide, aluminum oxide and aluminium nitride respectively
Beginning raw materials of compound, and weigh the cosolvent HBO of gross mass 4%3;
S2), it is put into corundum crucible after being ground the raw material in step S1), then crucible is put into high-temperature electric resistance furnace
Pre-burning in air atmosphere, pre-burning 2h under conditions of temperature is 700 DEG C;
S3), the sample after the pre-burning in step S2) is taken out, crucible is put into after being ground, in 5% H2With 95%
N2Mixing reducing atmosphere under 1400 DEG C calcination 5 hours;
S4), the sample after calcination in step S3) is taken out, with furnace natural cooling, obtains blue-green fluorescent after being ground
Powder, X-ray diffraction analysis show it for Sr4Al14O25Phase.
Embodiment 7
The sample that the present embodiment is prepared using Japan's Rigaku D/max-IIIA X-ray diffractometer measurement embodiment 1-6
Powder X-ray diffraction spectrum, test voltage 40kV, 1.2 °/min of scanning speed, test electric current 40mA, select Cu-K α 1X
Ray, wavelength areX-ray diffraction analysis shows it for Sr4Al14O25Phase, it is specific as shown in Figure 1,
Using the powder of 920 stable state of Edinburgh, Britain FLS and the sample of transient luminescence spectrometer measurement embodiment 1-4 preparation
The luminescent spectrum at end, xenon lamp power are 450 watts, and detector is the (work of Japan Hamamatsu refrigeration mode R928P photomultiplier tube
- 1250 volt of voltage), the data acquired integrated time is 0.2 second, scanning step 1nm, as shown in Fig. 2, as can be seen from Figure 2, sample exists
It can produce the blue green light that peak position is located at 490nm under 360nm excitation.And the powder of sample prepared by the present invention is tested using the above method
The relative luminous intensity that end changes with concentration, specifically as indicated at 3, it can be seen from the figure that the relative luminous intensity of fluorescent powder with
The increase of concentration and increase, as x=15%, the relative luminous intensity of fluorescent powder is best.
The above embodiments and description only illustrate the principle of the present invention and most preferred embodiment, is not departing from this
Under the premise of spirit and range, various changes and improvements may be made to the invention, these changes and improvements both fall within requirement and protect
In the scope of the invention of shield.
Claims (8)
1. a kind of method based on nitridation enhancing light-emitting phosphor intensity, it is characterised in that: replaced by introducing nitrogen part
Oxygen element realizes luminescence enhancement, and with strontium aluminate (Sr4Al14O25) it is used as luminescent ceramic matrix, Eu2+As luminescent activator,
HBO3As cosolvent, AlN enhancing is mixed in matrix and is shone, and blue-green fluorescent powder is synthesized using high temperature solid-state method
Sr3.96Eu0.04Al14-xAlxO25-xNx: xAlN, wherein 0%≤x≤25%.
2. a kind of method based on nitridation enhancing light-emitting phosphor intensity according to claim 1, it is characterised in that: use
High temperature solid-state method synthesizes blue-green fluorescent powder Sr3.96Eu0.04Al14-xAlxO25-xNx: xAlN specifically includes the following steps:
It S1), is Sr:Eu:Al:AlN=3.96:0.02:14-x:x according to molar ratio, wherein 0%≤x≤25%;It weighs respectively
Containing strontium, europium, aluminium compound raw material and aluminium nitride, and weigh the cosolvent HBO of all raw materials of compound quality 4%3;
S2), pre-burning in air atmosphere after being ground the raw material in step S1);
S3), after being ground the sample taking-up after the pre-burning in step S2), in H2Or N2Mixing reducing atmosphere or carbon reduction
Calcination under atmosphere;
S4), the sample after calcination in step S3) is taken out, blue-green fluorescent powder Sr is obtained after being ground3.96Eu0.04Al14- xAlxO25-xNx: xAlN, wherein 0%≤x≤25%.
3. a kind of method based on nitridation enhancing light-emitting phosphor intensity according to claim 2, it is characterised in that: step
S1 in), the raw materials of compound containing strontium is strontium carbonate or strontium nitrate.
4. a kind of method based on nitridation enhancing light-emitting phosphor intensity according to claim 2, it is characterised in that: step
S1 in), the raw materials of compound containing europium is europiumsesquioxide.
5. a kind of method based on nitridation enhancing light-emitting phosphor intensity according to claim 2, it is characterised in that: step
S1 in), the raw materials of compound of the aluminium is aluminium hydroxide or aluminum oxide.
6. a kind of method based on nitridation enhancing light-emitting phosphor intensity according to claim 2, it is characterised in that: step
S1 in), the x=15%.
7. a kind of method based on nitridation enhancing light-emitting phosphor intensity according to claim 2, it is characterised in that: step
S2 in), calcined temperature is 700 DEG C, and soaking time is 2 hours.
8. a kind of method based on nitridation enhancing light-emitting phosphor intensity according to claim 2, it is characterised in that: step
S3 in), calcination temperature is 1400 DEG C, and soaking time is 5 hours.
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CN114045169A (en) * | 2021-11-23 | 2022-02-15 | 光源股份有限公司 | Red fluorescent powder capable of being compounded with LED blue light chip into plant growth lamp and preparation method thereof |
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CN112961677A (en) * | 2021-02-03 | 2021-06-15 | 杭州电子科技大学 | Broadband near-infrared emission fluorescent powder capable of being excited by blue light and preparation method thereof |
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CN114045169A (en) * | 2021-11-23 | 2022-02-15 | 光源股份有限公司 | Red fluorescent powder capable of being compounded with LED blue light chip into plant growth lamp and preparation method thereof |
CN114045169B (en) * | 2021-11-23 | 2023-07-25 | 光源股份有限公司 | Red fluorescent powder capable of being compounded with LED blue light chip into plant growth lamp and preparation method thereof |
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Application publication date: 20190614 |