CN104694127A - Red fluorescent powder and preparation method thereof - Google Patents

Red fluorescent powder and preparation method thereof Download PDF

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Publication number
CN104694127A
CN104694127A CN201410826864.9A CN201410826864A CN104694127A CN 104694127 A CN104694127 A CN 104694127A CN 201410826864 A CN201410826864 A CN 201410826864A CN 104694127 A CN104694127 A CN 104694127A
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preparation
red fluorescence
fluorescence powder
xeu
nala
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CN201410826864.9A
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史永胜
陈思秋
宁青菊
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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Priority to CN201410826864.9A priority Critical patent/CN104694127A/en
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Abstract

The invention discloses red fluorescent powder and a preparation method thereof. The preparation method comprises the following steps: by selecting commercially available Na2CO3, La2O3, TeO2, Mg(NO3)2.6H2O and Eu2O3 as reaction raw materials, weighing all the raw materials according to the stoichiometric ratio in the chemical formula of NaLa1-xMgTeO6: xEu<3+>, wherein x is 0.01-0.11; the sintering temperature of the preparation process disclosed by the invention is relatively low and the process is simple; prepared NaLa1-xMgTeO6: xEu<3+> has regular appearance and uniform particle size distribution, and prepared NaLa[1-x]MgTeO6: xEu<3+> has very strong red light emission when subjected to excitation of 360nm ultraviolet light and high quantum conversion rate.

Description

Red fluorescence powder and preparation method thereof
Technical field
The invention belongs to fluorescent material field, relate to red fluorescence powder and preparation method thereof, particularly relate to a kind of NaLaMgTeO 6single rare earth doped Eu 3+ion fluorescent material realizing red emission and preparation method thereof.
Background technology
Luminescent material is generally made up of substrate material and activator ion.To Eu 3+, its 5d → 4f transition has broadband emission, and under different matrix, under the acting in conjunction of crystal field and electronic cloud expansion effect, its emmission spectrum can extend to infrared light district from ultraviolet region, is thus suitable as LED fluorescent material activator.To a certain extent, matrix group paired fluorescent mealiness can play a decisive role, and any substrate composed change all likely causes the change of crystal field strength, energy transfer process, finally has influence on luminous efficiency and the characteristics of luminescence of fluorescent material.
Current commercial white light LEDs principle mostly is blue light and gold-tinted compound obtains white light emission, and because it lacks red spectral components, cause light source colour rendering index lower, colour temperature is high.The three primary colors fluorescent powder recombined white light mode of recent research, its problem is the low and low lightness of the efficiency of conversion of red fluorescence powder, is difficult to the application requiring meeting high performance device, and therefore, the red fluorescence powder that development luminous intensity is higher becomes focus.
Tellurate is used for preparing glass optical fiber, and the application in fluorescent material field is little, and the present invention takes NaLaMgTeO 6as substrate material, a kind of NaLaMgTeO is prepared in design 6: Eu 3+new LED photoelectric material, this kind of fluorescent material yet there are no report.
Summary of the invention
The object of this invention is to provide a kind of red fluorescence powder and preparation method thereof, it takes NaLaMgTeO 6as substrate material, there is luminous intensity high, the feature of stable in properties.
The present invention solves above-mentioned technical problem by following technical proposals: a kind of red fluorescence powder, and its chemical constitution is NaLa 1-xmgTeO 6: xEu 3+, wherein x=0.01 ~ 0.11.
For solving the problem, present invention also offers a kind of preparation method of red fluorescence powder, concrete grammar is as follows:
1) commercially available Na is chosen 2cO 3, La 2o 3, TeO 2, Mg (NO 3) 26H 2o and Eu 2o 3as reaction raw materials, according to chemical formula NaLa 1-xmgTeO 6: xEu 3+stoichiometric ratio take each raw material, wherein x=0.01 ~ 0.11;
2) by step 1) in institute raw materials weighing put into ball mill, adopt dry mill process, setting speed 100 ~ 180r/min, carries out abundant agitation grinding and obtains mixture;
3) by step 2) in mixture after ball grinding stirring carry out solid state sintering, the system of solid state sintering is for from room temperature, 300 DEG C are risen to the speed of 2 ~ 3 DEG C/min, after with the ramp to 1100 of 3 ~ 5 DEG C/min DEG C ~ 1200 DEG C, insulation 3 ~ 7h, is then cooled to room temperature and obtains red fluorescence powder of the present invention.
Described step 3) solid state sintering mentioned is that mixture is put into corundum crucible, corundum crucible is placed in resistance furnace and sinters.
Described resistance furnace adopts chamber type electric resistance furnace.
Step 3) described in be cooled to stove naturally cooling.
Compared with prior art, the present invention at least has the following advantages: the sintering temperature of preparation technology of the present invention is lower, and technique is simple; The NaLa that the present invention prepares 1-xmgTeO 6: xEu 3+pattern rule, even particle size distribution, the NaLa that the present invention prepares 1-xmgTeO 6: xEu 3+there is when being subject to 360nm ultraviolet excitation very strong red emission, and quantum turnover ratio is high.The NaLa that the present invention prepares 1-xmgTeO 6: xEu 3+crystalline phase diffraction peak position is mated well with PDF standard card (NO.82-2366), can find out NaLa prepared by the present invention 1-xmgTeO 6: xEu 3+fluorescent material crystal property is good, and phase purity is higher.
And the present invention adopts dry mill process, without the need to the energy consumption of dry powder, greatly can save cost, simultaneously because do not produce waste water and the slag mud of rotating wash bowl grinding machine, also mitigate the pollution to empty G&W, and effectively shorten technical process, significantly improve production efficiency.
Accompanying drawing explanation
Fig. 1 is NaLa prepared by the present invention 1-xmgTeO 6: xEu 3+xRD figure.
Fig. 2 is NaLa prepared by the embodiment of the present invention 4 0.93mgTeO 6: 0.07Eu 3+the utilizing emitted light spectrogram of fluorescent material.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment 1:
1) commercially available Na is chosen 2cO 3, La 2o 3, TeO 2, Mg (NO 3) 26H 2o and Eu 2o 3as reaction raw materials, according to chemical formula NaLa 0.99mgTeO 6: 0.01Eu 3+stoichiometric ratio take each raw material;
2) institute's raw materials weighing is put into ball mill, adopt dry mill process, setting speed 100r/min, carries out abundant agitation grinding;
3) mixture after ball grinding stirring is put into corundum crucible, corundum crucible is placed in High Temperature Furnaces Heating Apparatus, rises to 300 DEG C with the speed of 3 DEG C/min, after with the ramp to 1200 DEG C of 5 DEG C/min, insulation 5h, is then cooled to room temperature and obtains red fluorescence powder NaLa of the present invention 0.99mgTeO 6: 0.01Eu 3+.
Embodiment 2:
1) commercially available Na is chosen 2cO 3, La 2o 3, TeO 2, Mg (NO 3) 26H 2o and Eu 2o 3as reaction raw materials, according to chemical formula NaLa 0.97mgTeO 6: 0.03Eu 3+stoichiometric ratio take each raw material.
2) institute's raw materials weighing is put into ball mill, adopt dry mill process, setting speed 120r/min, carries out abundant agitation grinding.
3) mixture after ball grinding stirring is put into corundum crucible, corundum crucible is placed in High Temperature Furnaces Heating Apparatus, rises to 300 DEG C with the speed of 2 DEG C/min, after with the ramp to 1200 DEG C of 4 DEG C/min, insulation 7h, is then cooled to room temperature and obtains red fluorescence powder NaLa of the present invention 0.97mgTeO 6: 0.03Eu 3+.
Embodiment 3:
1) commercially available Na is chosen 2cO 3, La 2o 3, TeO 2, Mg (NO 3) 26H 2o and Eu 2o 3as reaction raw materials, according to chemical formula NaLa 0.95mgTeO 6: 0.05Eu 3+stoichiometric ratio take each raw material.
2) institute's raw materials weighing is put into ball mill, adopt dry mill process, setting speed 150r/min, carries out abundant agitation grinding.
3) mixture after ball grinding stirring is put into corundum crucible, corundum crucible is placed in High Temperature Furnaces Heating Apparatus, rises to 300 DEG C with the speed of 3 DEG C/min, after with the ramp to 1100 DEG C of 3 DEG C/min, insulation 3h, is then cooled to room temperature and obtains red fluorescence powder NaLa of the present invention 0.95mgTeO 6: 0.05Eu 3+.
Embodiment 4:
1) commercially available Na is chosen 2cO 3, La 2o 3, TeO 2, Mg (NO 3) 26H 2o and Eu 2o 3as reaction raw materials, according to chemical formula NaLa 0.93mgTeO 6: 0.07Eu 3+stoichiometric ratio take each raw material.
2) institute's raw materials weighing is put into ball mill, adopt dry mill process, setting speed 150r/min, carries out abundant agitation grinding.
3) mixture after ball grinding stirring is put into corundum crucible, corundum crucible is placed in High Temperature Furnaces Heating Apparatus, rises to 300 DEG C with the speed of 3 DEG C/min, after with the ramp to 1100 DEG C of 5 DEG C/min, insulation 4h, is then cooled to room temperature and obtains red fluorescence powder NaLa of the present invention 0.93mgTeO 6: 0.07Eu 3+.
Fig. 2 is NaLa 0.93mgTeO 6: 0.07Eu 3+the utilizing emitted light spectrogram that fluorescent material monitors under the exciting of 360nm near-ultraviolet light.Eu 3+ion enters NaLaMgTeO 6after lattice, under the exciting of near-ultraviolet light, present wide range multi-peak emission, emission peak lays respectively at 588nm, 629nm, 695nm place, covers whole red light region.
As shown in Figure 1, the NaLa for preparing of the present invention 1-xmgTeO 6: xEu 3+crystalline phase diffraction peak position is mated well with PDF standard card (NO.82-2366), can find out NaLa prepared by the present invention 1-xmgTeO 6: xEu 3+fluorescent material crystal property is good, and phase purity is higher.
Embodiment 5:
1) commercially available Na is chosen 2cO 3, La 2o 3, TeO 2, Mg (NO 3) 26H 2o and Eu 2o 3as reaction raw materials, according to chemical formula NaLa 0.89mgTeO 6: 0.11Eu 3+stoichiometric ratio take each raw material.
2) institute's raw materials weighing is put into ball mill, adopt dry mill process, setting speed 180r/min, carries out abundant agitation grinding.
3) mixture after ball grinding stirring is put into corundum crucible, corundum crucible is placed in High Temperature Furnaces Heating Apparatus, rises to 300 DEG C with the speed of 2 DEG C/min, after with the ramp to 1150 DEG C of 5 DEG C/min, insulation 7h, is then cooled to room temperature and obtains red fluorescence powder NaLa of the present invention 0.89mgTeO 6: 0.11Eu 3+.

Claims (5)

1. a red fluorescence powder, is characterized in that, its chemical constitution expression formula is NaLa 1-xmgTeO 6: xEu 3+, wherein x=0.01 ~ 0.11.
2. a preparation method for red fluorescence powder, is characterized in that, comprises the following steps:
1) commercially available Na is chosen 2cO 3, La 2o 3, TeO 2, Mg (NO 3) 26H 2o and Eu 2o 3as reaction raw materials, according to chemical formula NaLa 1-xmgTeO 6: xEu 3+stoichiometric ratio take each raw material, wherein x=0.01 ~ 0.11;
2) by step 1) in institute raw materials weighing put into ball mill, adopt dry mill process, setting speed 100 ~ 180r/min, carries out abundant agitation grinding and obtains mixture;
3) by step 2) in mixture after ball grinding stirring carry out solid state sintering, the system of solid state sintering is for from room temperature, 300 DEG C are risen to the speed of 2 ~ 3 DEG C/min, after with the ramp to 1100 of 3 ~ 5 DEG C/min DEG C ~ 1200 DEG C, insulation 3 ~ 7h, is then cooled to room temperature and obtains red fluorescence powder of the present invention.
3. the preparation method of a kind of red fluorescence powder according to claim 2, is characterized in that, described step 3) solid state sintering mentioned is that mixture is put into corundum crucible, corundum crucible is placed in resistance furnace and sinters.
4. the preparation method of a kind of red fluorescence powder according to claim 3, is characterized in that, described resistance furnace adopts chamber type electric resistance furnace.
5. the preparation method of a kind of red fluorescence powder according to claim 2, is characterized in that, step 3) described in be cooled to stove naturally cooling.
CN201410826864.9A 2014-12-25 2014-12-25 Red fluorescent powder and preparation method thereof Pending CN104694127A (en)

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Application Number Priority Date Filing Date Title
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3487025A (en) * 1966-09-14 1969-12-30 Gen Telephone & Elect Rare earth tellurate phosphors
CN102660289A (en) * 2012-05-04 2012-09-12 苏州大学 Europium ion Eu<3+> activated tellurate red luminescence fluorescent powder, preparation method and application
CN103788953A (en) * 2014-02-28 2014-05-14 淮南师范学院 Europium-activated tellurate red phosphor and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3487025A (en) * 1966-09-14 1969-12-30 Gen Telephone & Elect Rare earth tellurate phosphors
CN102660289A (en) * 2012-05-04 2012-09-12 苏州大学 Europium ion Eu<3+> activated tellurate red luminescence fluorescent powder, preparation method and application
CN103788953A (en) * 2014-02-28 2014-05-14 淮南师范学院 Europium-activated tellurate red phosphor and preparation method thereof

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