CN103881702A - Method for preparing Eu-doped Ca2Si5N8 red light emission fluorescent powder - Google Patents

Method for preparing Eu-doped Ca2Si5N8 red light emission fluorescent powder Download PDF

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CN103881702A
CN103881702A CN201410111797.2A CN201410111797A CN103881702A CN 103881702 A CN103881702 A CN 103881702A CN 201410111797 A CN201410111797 A CN 201410111797A CN 103881702 A CN103881702 A CN 103881702A
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祝迎春
汪洋
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Shanghai Institute of Ceramics of CAS
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Abstract

The invention relates to a method for preparing Eu-doped Ca2Si5N8 red light emission fluorescent powder. The method comprises the following steps: (1) weighing raw materials, including a calcium source, Si3N4 serving as a silicon source and Eu2O3 serving as an europium source in the molar ratio of Ca to Si to Eu being 2:5:(0.02-0.5), grinding, and uniformly mixing into a powder raw material, wherein the calcium source comprises a first calcium source containing at least one of CaO, Ca(OH2) and CaCO3, and a second calcium source of Ca(CH3COO)2 also serving as a reducing agent; (2) preserving heat of the obtained powder raw material under nitrogen gas current at the temperature of 1500-2300K for 0.5-4 hours, and sintering to obtain sintered blocks; (3) grinding the obtained sintered blocks into uniform powder to obtain the Eu-doped Ca2Si5N8 red light emission fluorescent powder. In the method, the adopted calcium source includes Ca(CH3COO)2 which is also taken as the reducing agent, so that other reducing agents do not need to be used.

Description

One is prepared Eu doping Ca 2si 5n 8the method of red-light fluorescent powder
Technical field
The present invention relates to a kind of use acetate to do reductive agent high temperature solid-state method to prepare Eu doping Ca 2si 5n 8the method of red-light fluorescent powder, belongs to materials chemistry field.
Background technology
Compared with traditional lighting light source, white light LEDs has the advantages such as volume is little, less energy consumption, response is fast, the life-span is long, be therefore described as the 4th generation lighting source.The colour rendering index (Ra) of business white light LEDs can reach 85 at present, can realize cold white or color of sunshine illumination, enough as general illumination, but also lack ruddiness and low colour temperature district color developing is bad, be difficult to realize the warm white of low colour temperature, high-color rendering, and biomedical and building lighting light source need warm white.Existing yellow emission and red emission material are little, and some also contains the toxic ingredients such as sulphur, chlorine, cadmium, or easily deliquescence, poor heat stability, require hydrolysis to carry out complicated processing, and these greatly reduce the output quality of light and the life-span of LED.In order to overcome above problem, need to develop a kind of novel material with efficient, high stability and non-environmental-pollution.The excitation wavelength of conventional oxide luminescent material is positioned at ultraviolet region, and rear-earth-doped silicon nitride, nitrogen-atoms covalency obviously strengthens, thereby make it have some special optical properties, as excitation band, visible region has been arrived in red shift,, just in time mates with the emission wavelength of near ultraviolet and blue light diode to the strong absorption in blue area near ultraviolet region, so be to prepare the substrate material that white light LEDs is suitable, wherein Ca 2si 5n 8it is exactly so a kind of material.Ca at present 2si 5n 8mainly contain nitrogenize solid reaction process, atmosphere reduction method, carbothermic method several, every kind of method all exists some shortcomings, wherein nitrogenize solid reaction process preparation process complexity, and wayward, cost is high, yields poorly; The preparation of atmosphere reduction method raw material is complicated, and fluorescent material purity is wayward; In carbothermic method, remaining carbon dust has a strong impact on energy absorption and the light emission of fluorescent material.
Summary of the invention
In the face of the problem that prior art exists, the object of the present invention is to provide a kind of high temperature solid-state method to prepare Ca 2si 5n 8the method of red-light fluorescent powder.
At this, the invention provides one and prepare Eu doping Ca 2si 5n 8the method of red-light fluorescent powder, comprising:
(1) Ca:Si:Eu=2:5:(0.02～0.5 in molar ratio) ratio take calcium source, Si as silicon source 3n 4, and as the Eu in europium source 2o 3for raw material ground and mixed are evenly powder raw material, wherein said calcium source comprises contains CaO, Ca (OH) 2, and CaCO 3in at least one the first calcium source and double as the Ca (CH into reductive agent 3cOO) 2the second calcium source;
(2) gained powder raw material is carried out to sintering for 0.5～4 hour in 1500K～2300K insulation under stream of nitrogen gas and obtain sintering block; And
(3) gained sintering block is ground to form to uniformed powder, make europium doping Ca 2si 5n 8red-light fluorescent powder.
In the present invention, the calcium source adopting comprises Ca (CH 3cOO) 2, it can be simultaneously as reductive agent, thereby without re-using other reductive agent.Method of the present invention and preparation Ca 2si 5n 8the common methods of fluorescent material is compared as nitrogenize solid reaction process, atmosphere reduction method, carbothermic method, prepares required starting material and very easily obtains and low price, can greatly reduce costs; Preparation process is few, and method is easy, consuming time short, very efficiently convenient; Making product does not have reaction raw materials remnants, and composition is pure.
Preferably, in described calcium source, the mol ratio in described the second calcium source and described the first calcium source is greater than 1:8.
Preferably, in step (1), the preparation of described powder raw material comprises: in described raw material, add the grinding medium of 0.5～20 times of volume, be ground to and mix; And within 0.5～24 hour, be dried to make powder raw material in 40～160 ℃ of insulations.
Preferably, described grinding medium is alcohol and/or acetone.
Preferably, in step (1), the preparation of described powder raw material also comprises: the raw material because of described dry and soft-agglomerated is ground to form to uniformed powder again.
Preferably, in step (2), temperature when sintering is to rise to 1500K～2300K from room temperature in 5 minutes.
Preferably, in step (2), stream of nitrogen gas amount is 0.01～1000mL/ minute.
Accompanying drawing explanation
Fig. 1 is Ca 1.98si 5n 8: Eu 0.02xRD figure picture and standard C a 2si 5n 8the comparison diagram of XRD figure picture;
Fig. 2 is Ca 1.98si 5n 8: Eu 0.02sEM scan image;
Fig. 3 is Ca 1.98si 5n 8: Eu 0.02emmission spectrum under different excitation wavelengths;
Fig. 4 is the mol ratio in the first calcium source and the second calcium source 420nm excitation wavelength emmission spectrum under exciting while being 1:2,2:3,1:1,3:2.
Embodiment
Further illustrate the present invention below in conjunction with accompanying drawing and following embodiment, should be understood that accompanying drawing and following embodiment are only for the present invention is described, and unrestricted the present invention.
The invention provides a kind of high temperature solid-state method and prepare Eu doping Ca 2si 5n 8the method of red-light fluorescent powder, with CaO, Ca (OH) 2, and CaCO 3in at least one, Ca (CH 3cOO) 2, silicon nitride, europium sesquioxide be raw material, Ca (CH 3cOO) 2serve as reductive agent simultaneously, prepare Ca by high temperature solid-state method 2si 5n 8red-light fluorescent powder.Particularly, as example, method of the present invention can comprise the following steps.
(1) Ca:Si:Eu=2:5:(0.02～0.5 in molar ratio) ratio to take calcium source, silicon source, europium source be raw material, and be ground to and mix.Wherein, the calcium source adopting can comprise CaO, the Ca (OH) as the first calcium source 2, and/or CaCO 3, and as the Ca (CH of the second calcium source while as reductive agent 3cOO) 2.The mol ratio in the second calcium source and the first calcium source can be greater than 1:8.CaO, Ca (OH) in the first calcium source 2, and/or CaCO 3it can be arbitrary proportion.The silicon source adopting includes but not limited to Si 3n 4.The europium source adopting includes but not limited to Eu 2o 3.The grinding medium (for example alcohol and/or acetone) that can add 0.5～20 times of raw material volume in grinding is ground to and mixes in mortar.In addition, above adopted raw material and chemical reagent can be analytical pure and above purity.
(2) raw material mixing in step (1) is dried, the loft drier of for example putting into 40～160 ℃ is extremely dried for 2～4 hours.
(3) if step (2) Raw, because of dry and soft-agglomerated, can grind to form uniformed powder again in grinding.Should be understood that this step is not essential, soft-agglomerated if step (2) Raw does not occur, without carrying out this step.
(4) powder raw material obtaining in step (3) is carried out to sintering for 0.5～4 hour in 1500K～2300K insulation under stream of nitrogen gas and make sintering block.In one example, powder raw material is for example added, in high temperature resistant reaction vessel (graphite or boron nitride crucible), put into airtight heating unit (for example high frequency furnace), after vacuumizing, pass into nitrogen to opening air outlet valve with outer normal atmosphere balance, and in reaction process, continuing to pass into nitrogen assurance stream of nitrogen gas, airshed can be 0.01～1000mL/ minute.After nitrogen gas stream is stable, open high frequency furnace temperature was risen to 1500K～2300K from room temperature in 5 minutes, keep this temperature to slowly cool to room temperature after 0.5～4 hour.
(5) sintering block step (4) being obtained is put into mortar and is ground to form uniformed powder, makes Eu doping Ca 2si 5n 8red-light fluorescent powder.
Fig. 1 illustrates the Ca of prepared in accordance with the method for the present invention 1.98si 5n 8: Eu 0.02xRD figure picture and standard C a 2si 5n 8the comparison diagram of XRD figure picture, as shown in Figure 1, makes powder peak position and mates with standard card peak position, and making powder is really Ca 2si 5n 8.Fig. 2 illustrates Ca 1.98si 5n 8: Eu 0.02sEM scan image, as shown in Figure 2, making morphology microstructure is the little crystal grain of sintering.Fig. 3 illustrates Ca 1.98si 5n 8: Eu 0.02emmission spectrum under different excitation wavelengths, as shown in Figure 3, the excitation peak that makes powder is blue region in 420nm left and right.The emmission spectrum of 420nm excitation wavelength under exciting when Fig. 4 illustrates the mol ratio that adopts different the first calcium source and the second calcium source, as shown in Figure 4, the emission peak that makes powder is orange red light at 594nm.
Method of the present invention and preparation Ca 2si 5n 8the common methods of fluorescent material is compared and is had following advantage as nitrogenize solid reaction process, atmosphere reduction method, carbothermic method:
The required starting material of 1 preparation very easily obtain and low price, can greatly reduce costs;
2 preparation processes are few, and method is easy, consuming time short, very efficiently convenient;
3 make product does not have reaction raw materials remnants, and composition is pure.
Further exemplify embodiment below to describe the present invention in detail.Should understand equally; following examples are only used to further illustrate the present invention; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.The processing parameter that following example is concrete etc. is only also an example in OK range, and those skilled in the art can be done in suitable scope and be selected by explanation herein, and do not really want to be defined in the below concrete numerical value of example.
Embodiment 1
(1) ratio of Ca:Si:Eu=2:5:0.02 takes the CaCO as calcium source in molar ratio 3, Ca (CH 3cOO) 2(n (CaCO 3): n (Ca (CH 3cOO) 2)=3:2), as the Si in silicon source 3n 4, as the Eu in europium source 2o 3for raw material, and add alcohol or the acetone of 2 times of raw material volumes to do grinding medium, in mortar, be ground to and mix;
(2) raw material mixing in step (1) is put into the loft drier 2～4 hours of 80 ℃ to dry;
(3) by step (2) because dry and soft-agglomerated raw material grinds to form uniformed powder again in mortar;
(4) powder raw material obtaining in step (3) is added in graphite or boron nitride crucible, put into high frequency furnace, after vacuumizing, pass into nitrogen to opening air outlet valve with outer normal atmosphere balance, and continue to pass into nitrogen assurance stream of nitrogen gas with the flow of 300mL/ minute in reaction process;
(5) after nitrogen gas stream is stable, opens high frequency furnace temperature was risen to 1500K～2000K from room temperature in 5 minutes, keep this temperature to slowly cool to room temperature after 1～2 hour;
(6) sintering block step (5) being obtained is put into mortar and is ground to form uniformed powder.Its emmission spectrum under 420nm excitation wavelength excites is referring to Fig. 4.
Embodiment 2
(1) ratio of Ca:Si:Eu=2:5:0.02 takes the CaCO as calcium source in molar ratio 3, Ca (CH 3cOO) 2(n (CaCO 3): n (Ca (CH 3cOO) 2)=1:1), as the Si in silicon source 3n 4, as the Eu in europium source 2o 3for raw material, and add alcohol or the acetone of 2 times of raw material volumes to do grinding medium, in mortar, be ground to and mix;
(2) raw material mixing in step (1) is put into the loft drier 2～4 hours of 80 ℃ to dry;
(3) by step (2) because dry and soft-agglomerated raw material grinds to form uniformed powder again in mortar;
(4) powder raw material obtaining in step (3) is added in graphite or boron nitride crucible, put into high frequency furnace, after vacuumizing, pass into nitrogen to opening air outlet valve with outer normal atmosphere balance, and continue to pass into nitrogen assurance stream of nitrogen gas with the flow of 100mL/ minute in reaction process;
(5) after nitrogen gas stream is stable, opens high frequency furnace temperature was risen to 1500K～2000K from room temperature in 5 minutes, keep this temperature to slowly cool to room temperature after 1～2 hour;
(6) sintering block step (5) being obtained is put into mortar and is ground to form uniformed powder.Its emmission spectrum under 420nm excitation wavelength excites is referring to Fig. 4.
Embodiment 3
(1) ratio of Ca:Si:Eu=2:5:0.02 takes the CaCO as calcium source in molar ratio 3, Ca (CH 3cOO) 2(n (CaCO 3): n (Ca (CH 3cOO) 2)=2:3), as the Si in silicon source 3n 4, as the Eu in europium source 2o 3for raw material, and add alcohol or the acetone of 2 times of raw material volumes to do grinding medium, in mortar, be ground to and mix;
(2) raw material mixing in step (1) is put into the loft drier 2～4 hours of 80 ℃ to dry;
(3) by step (2) because dry and soft-agglomerated raw material grinds to form uniformed powder again in mortar;
(4) powder raw material obtaining in step (3) is added in graphite or boron nitride crucible, put into high frequency furnace, after vacuumizing, pass into nitrogen to opening air outlet valve with outer normal atmosphere balance, and continue to pass into nitrogen assurance stream of nitrogen gas with the flow of 400mL/ minute in reaction process;
(5) after nitrogen gas stream is stable, opens high frequency furnace temperature was risen to 1500K～2000K from room temperature in 5 minutes, keep this temperature to slowly cool to room temperature after 1～2 hour;
(6) sintering block step (5) being obtained is put into mortar and is ground to form uniformed powder, makes Ca 1.98si 5n 8: Eu 0.02powder.Its XRD figure picture, SEM scan image, emmission spectrum under different excitation wavelengths are respectively referring to Fig. 1,2,3, and its emmission spectrum under 420nm excitation wavelength excites is referring to Fig. 4.
Embodiment 4
(1) ratio of Ca:Si:Eu=2:5:0.02 takes the CaCO as calcium source in molar ratio 3, Ca (CH 3cOO) 2(n (CaCO 3): n (Ca (CH 3cOO) 2)=1:2), as the Si in silicon source 3n 4, as the Eu in europium source 2o 3for raw material, and add alcohol or the acetone of 2 times of raw material volumes to do grinding medium, in mortar, be ground to and mix;
(2) raw material mixing in step (1) is put into the loft drier 2～4 hours of 40 ℃ to dry;
(3) by step (2) because dry and soft-agglomerated raw material grinds to form uniformed powder again in mortar;
(4) powder raw material obtaining in step (3) is added in graphite or boron nitride crucible, put into high frequency furnace, after vacuumizing, pass into nitrogen to opening air outlet valve with outer normal atmosphere balance, and continue to pass into nitrogen assurance stream of nitrogen gas with the flow of 800mL/ minute in reaction process;
(5) after nitrogen gas stream is stable, opens high frequency furnace temperature was risen to 1500K～2300K from room temperature in 5 minutes, keep this temperature to slowly cool to room temperature after 1～2 hour;
(6) sintering block step (5) being obtained is put into mortar and is ground to form uniformed powder.Its emmission spectrum under 420nm excitation wavelength excites is referring to Fig. 4.
Embodiment 5
(1) ratio of Ca:Si:Eu=2:5:0.4 takes CaO, the Ca (CH as calcium source in molar ratio 3cOO) 2(n (CaO): n (Ca (CH 3cOO) 2)=7:1), as the Si in silicon source 3n 4, as the Eu in europium source 2o 3for raw material, and add alcohol or the acetone of 2 times of raw material volumes to do grinding medium, in mortar, be ground to and mix;
(2) raw material mixing in step (1) is put into the loft drier 2～4 hours of 80 ℃ to dry;
(3) by step (2) because dry and soft-agglomerated raw material grinds to form uniformed powder again in mortar;
(4) powder raw material obtaining in step (3) is added in graphite or boron nitride crucible, put into high frequency furnace, after vacuumizing, pass into nitrogen to opening air outlet valve with outer normal atmosphere balance, and continue to pass into nitrogen assurance stream of nitrogen gas with the flow of 50mL/ minute in reaction process;
(5) after nitrogen gas stream is stable, opens high frequency furnace temperature was risen to 1500K～2000K from room temperature in 5 minutes, keep this temperature to slowly cool to room temperature after 1～2 hour;
(6) sintering block step (5) being obtained is put into mortar and is ground to form uniformed powder.
Embodiment 6
(1) ratio of Ca:Si:Eu=2:5:0.1 takes the Ca (OH) as calcium source in molar ratio 2, Ca (CH 3cOO) 2(n (Ca (OH) 2): n (Ca (CH 3cOO) 2)=1:1), as the Si in silicon source 3n 4, as the Eu in europium source 2o 3for raw material, and add alcohol or the acetone of 2 times of raw material volumes to do grinding medium, in mortar, be ground to and mix;
(2) raw material mixing in step (1) is put into the loft drier 2～4 hours of 160 ℃ to dry;
(3) by step (2) because dry and soft-agglomerated raw material grinds to form uniformed powder again in mortar;
(4) powder raw material obtaining in step (3) is added in graphite or boron nitride crucible, put into high frequency furnace, after vacuumizing, pass into nitrogen to opening air outlet valve with outer normal atmosphere balance, and continue to pass into nitrogen assurance stream of nitrogen gas with the flow of 1000mL/ minute in reaction process;
(5) after nitrogen gas stream is stable, opens high frequency furnace temperature was risen to 1500K～2000K from room temperature in 5 minutes, keep this temperature to slowly cool to room temperature after 1～2 hour;
(6) sintering block step (5) being obtained is put into mortar and is ground to form uniformed powder.
Industrial applicability: method of the present invention have cost low, react the advantage such as fast, simple to operate, product is pure, have great application prospect in fields such as white light LEDs.

Claims (7)

1. prepare Eu doping Ca for one kind 2si 5n 8the method of red-light fluorescent powder, is characterized in that, comprising:
(1) Ca:Si:Eu=2:5:(0.02～0.5 in molar ratio) ratio take calcium source, Si as silicon source 3n 4, and as the Eu in europium source 2o 3for raw material ground and mixed are evenly powder raw material, wherein said calcium source comprises contains CaO, Ca (OH) 2, and CaCO 3in at least one the first calcium source and double as the Ca (CH into reductive agent 3cOO) 2the second calcium source;
(2) gained powder raw material is carried out to sintering for 0.5～4 hour in 1500K～2300K insulation under stream of nitrogen gas and obtain sintering block; And
(3) gained sintering block is ground to form to uniformed powder, make europium doping Ca 2si 5n 8red-light fluorescent powder.
2. method according to claim 1, is characterized in that, in described calcium source, the mol ratio in described the second calcium source and described the first calcium source is greater than 1:8.
3. method according to claim 1 and 2, is characterized in that, in step (1), the preparation of described powder raw material comprises: in described raw material, add the grinding medium of 0.5～20 times of volume, be ground to and mix; And within 0.5～24 hour, be dried to make powder raw material in 40～160 ℃ of insulations.
4. method according to claim 3, is characterized in that, described grinding medium is alcohol and/or acetone.
5. according to the method described in claim 3 or 4, it is characterized in that, in step (1), the preparation of described powder raw material also comprises: the raw material because of described dry and soft-agglomerated is ground to form to uniformed powder again.
6. according to the method described in any one in claim 1 to 5, it is characterized in that, in step (2), temperature when sintering is to rise to 1500K～2300K from room temperature in 5 minutes.
7. according to the method described in any one in claim 1 to 6, it is characterized in that, in step (2), stream of nitrogen gas amount is 0.01～1000mL/ minute.
CN201410111797.2A 2014-03-24 2014-03-24 Method for preparing Eu-doped Ca2Si5N8 red light emission fluorescent powder Pending CN103881702A (en)

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Application publication date: 20140625