CN104073252A - Preparation method of ZnB2O4:Eu<3+> luminescent material - Google Patents

Preparation method of ZnB2O4:Eu<3+> luminescent material Download PDF

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CN104073252A
CN104073252A CN201410249971.XA CN201410249971A CN104073252A CN 104073252 A CN104073252 A CN 104073252A CN 201410249971 A CN201410249971 A CN 201410249971A CN 104073252 A CN104073252 A CN 104073252A
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luminescent material
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CN104073252B (en
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刘志宏
乔丽钧
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Shaanxi Normal University
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Shaanxi Normal University
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Abstract

The invention discloses a preparation method of a ZnB2O4:Eu<3+> luminescent material. The preparation method comprises the steps of with ZnSO4.7H2O, Na2B4O7.10H2O and Eu2O3 as raw materials, uniformly mixing the raw materials, and then, carrying out one-step synthesis at room temperature to obtain Zn[B3O3(OH)5]H2O:Eu<3+>; roasting obtained Zn[B3O3(OH)5]H2O:Eu<3+> at high temperature for phase conversion to obtain the ZnB2O4: Eu<3+> luminescent material. The preparation method disclosed by the invention is easily-obtained in raw materials, simple in step and capable of rapidly and effectively preparing the ZnB2O4:Eu<3+> luminescent material; in addition, the ZnB2O4:Eu<3+> luminescent material obtained by using the preparation method disclosed by the invention is small in particle size and higher in luminescent intensity as comparison with the ZnB2O4:Eu<3+> luminescent material prepared by using the traditional high-temperature solid-phase method and wide in application to different fields such as display, light sources, medicines and the like.

Description

ZnB 2o 4: Eu 3+the preparation method of luminescent material
Technical field
The present invention relates to a kind of preparation method of luminescent material, relate to specifically ZnB 2o 4: Eu 3+the preparation method of luminescent material, belongs to chemical field.
Background technology
ZnB 2o 4: Eu 3+luminescent material is a kind of novel borate substrate luminescent material of development in recent years, be that substrate luminescent material is compared with traditional silicate, aluminate and phosphoric acid salt, there is more stable chemical property, and color developing is good, luminous efficiency is high, in the different field such as demonstration video picture, light source, photoelectronics, medical science, oneself has obtained utilizing widely.
The research of existing borate salt system luminescent material, has obtained certain progress at aspects such as its synthetic method, luminescent properties, luminescence mechanisms.Aspect synthetic method, prior art is mainly by the synthetic different types of borate substrate luminescent material of the method such as high temperature solid-state method, sol-gel method, wherein high temperature solid-state method is to prepare at present the most frequently used method of these anhydrous borate substrate luminescent materials, and common matrix is: rare-earth borate, alkaline earth metal borate, rare earth and alkaline-earth metal Composite borate and binary rare-earth metal perborate base status.
Specific to ZnB 2o 4: Eu 3+luminescent material, current preparation method adopts traditional high temperature solid-state method, with zinc oxide (ZnO), boric acid (H 3bO 3) and europium sesquioxide (Eu 2o 3) for high-temperature roasting after raw material mixed grinding obtains, the product purity that this preparation method obtains is not high, reunites serious, pattern, particle diameter are wayward, and crucial is the luminous intensity deficiency of products obtained therefrom, is difficult to meet the actual needs in each field.
Summary of the invention
For the defect of prior art, the present patent application people is by studying for a long period of time, fully studied different material, differential responses path is used for preparing ZnB 2o 4: Eu 3+the impact of luminescent material on its productive rate, purity, luminous intensity etc., in a large amount of raw materials and reflection path the pleasantly surprised discovery of applicant the ZnB that obtains of a kind of thermal transition preparation method 2o 4: Eu 3+luminescent material has the advantages that particle diameter is little, purity is high and luminous intensity is high.
Based on above-mentioned discovery, applicant has completed technical scheme of the present invention.The present invention is achieved through the following technical solutions:
ZnB 2o 4: Eu 3+the preparation method of luminescent material, comprises the steps:
1) with ZnSO 47H 2o, Na 2b 4o 710H 2o and Eu 2o 3mix one-step synthesis and obtain Zn[B for raw material is added to the water 3o 3(OH) 5] H 2o:Eu 3+;
2) by gained Zn[B 3o 3(OH) 5] H 2o:Eu 3+at high temperature roasting inversion of phases obtains ZnB 2o 4: Eu 3+luminescent material.
In preparation method, in order to reduce the interference of foreign metal ion pair reaction process, water used is preferably distilled water, more preferably redistilled water.The purified water of other type, for example deionized water, ultrapure water, be also obviously can be for of the present invention.
In technical scheme of the present invention, step 1) each raw material consumption and reaction conditions can select as required, in order to reduce wastage of material, improve resultant velocity, applicant's broad research the impact of the raw material proportion of composing on different amounts under various reaction conditionss, find to there is in the following cases good combined coefficient:
Step 1) ZnSO used 47H 2o, Na 2b 4o 710H 2o, Eu 2o 3, water mol ratio be 1: 0.5～3: 0.01～0.10: 250～550, reaction conditions is stirring reaction 12～72 hours under room temperature.
Preferably, ZnSO 47H 2o, Na 2b 4o 710H 2o, Eu 2o 3, water mol ratio be 1: 0.5～1.5: 0.03～0.08: 250～550, reaction conditions is stirring reaction 24～72 hours under room temperature.
Most preferred, ZnSO 47H 2o, Na 2b 4o 710H 2o, Eu 2o 3, water mol ratio be 1: 1: 0.06: 450, under room temperature, react 48 hours.
In above-mentioned, alleged room temperature, adopts routine cognition chemically, 20～25 DEG C.
In above-mentioned, in order to improve speed of reaction, each raw material is fully contacted, in room temperature reaction process, continue to stir.
Wherein, stirring velocity and alr mode are that working condition and the instrument that those skilled in the art adopt according to reality can be selected, and normally adopt stirrer, stirred autoclave etc. to stir with the speed of 100-2000r/min.
In above-mentioned, in order to improve product purity, to reduce impurity, and be convenient to step 2) operation, also comprise reaction product suction filtration, washing, dry step.
In technical scheme of the present invention, step 2) make step 1 by high-temperature calcination) reaction product fully there is thermal transition, i.e. Zn[B 3o 3(OH) 5] H 2o:Eu 3+change into ZnB 2o 4: Eu 3+luminescent material.
Wherein, step 2) temperature and calcination time be not subject to special restriction, as long as make it that thermal transition occur, preferred steps 2) then cooling 700～1000 DEG C of roastings 3～9 hours, more preferably step 2) then cooling 800～1000 DEG C of roastings 3～9 hours, most preferably step 2) then cooling 900 DEG C of roastings 6 hours.
Adopt above-mentioned preparation process, technique of the present invention not only raw material sources is easy to get, and reaction process step is simple, thereby has reduced production cost, improves product purity, the more important thing is the ZnB that adopts preparation method of the present invention to obtain 2o 4: Eu 3+luminescent material particle diameter is little, and its median size is at 1 micron, and concentration degree is high, and size is substantially impartial, makes it have the ZnB preparing than conventional high-temperature solid phase method 2o 4: Eu 3+the luminous intensity that luminescent material is higher, thus be widely used in showing the different field such as video picture, light source, medical science.
Brief description of the drawings
Fig. 1 is Zn[B prepared by embodiment 1 3o 3(OH) 5] H 2o:Eu 3+x ray energy dispersion spectrogram.
Fig. 2 a is ZnB prepared by embodiment 1 2o 4: Eu 3+the X ray energy dispersion spectrogram of luminescent material.
Fig. 2 b is ZnB prepared by comparative example 1 2o 4: Eu 3+the X ray energy dispersion spectrogram of luminescent material.
Fig. 3 is Zn[B prepared by embodiment 1 3o 3(OH) 5] H 2o:Eu 3+x-ray powder diffraction figure.
Fig. 4 a is ZnB prepared by embodiment 1 2o 4: Eu 3+the X-ray powder diffraction figure of luminescent material.
Fig. 4 b is ZnB prepared by comparative example 1 2o 4: Eu 3+the X-ray powder diffraction figure of luminescent material.
Fig. 5 a is ZnB prepared by embodiment 1 2o 4: Eu 3+the scanning electron microscope (SEM) photograph of luminescent material.
Fig. 5 b is ZnB prepared by comparative example 1 2o 4: Eu 3+the scanning electron microscope (SEM) photograph of luminescent material.
Fig. 6 is ZnB prepared by embodiment 1 2o 4: Eu 3+znB prepared by luminescent material (a) and comparative example's 1 high temperature solid-state method 2o 4: Eu 3+the utilizing emitted light spectrogram of luminescent material (b).
Embodiment
Embodiment 1
Step 1): preparation Zn[B 3o 3(OH) 5] H 2o:Eu 3+
By 2.87g ZnSO 47H 2o, 3.81g Na 2b 4o 710H 2o and 0.105g Eu 2o 3be dissolved in 80mL distilled water ZnSO 47H 2o and Na 2b 4o 710H 2o, Eu 2o 3the mol ratio of redistilled water is 1: 1: 0.06: 450, and stirring at room temperature 48 hours, by the separation of reaction product suction filtration, respectively washs 3 times with redistilled water and dehydrated alcohol respectively, is placed in interior 40 DEG C of baking oven and is dried 24 hours, obtains Zn[B 3o 3(OH) 5] H 2o:Eu 3+.
Step 2): preparation ZnB 2o 4: Eu 3+luminescent material
By step 1) Zn[B that obtains 3o 3(OH) 5] H 2o:Eu 3+900 DEG C of roastings 6 hours, cooling, obtain ZnB 2o 4: Eu 3+luminescent material.
Comparative example 1
Adopt conventional high-temperature solid phase method to prepare ZnB 2o 4: Eu 3+luminescent material, concrete grammar is: with ZnO, H 3bO 3and Eu 2o 3after raw material mixed grinding, ZnO and H 3bO 3, Eu 2o 3mol ratio be 1: 2.05: 0.03,900 DEG C of roastings 6 hours, obtain ZnB 2o 4: Eu 3+luminescent material.
On the basis of the above, the ZnB that applicant prepares preparation method of the present invention and traditional method 2o 4: Eu 3+the physicochemical property of luminescent material compares, and below in conjunction with accompanying drawing, experimental result is described:
(working conditions is: Cu target Ka line to adopt Rigaku D/MAX-IIIC type x-ray powder diffraction instrument, graphite flake filtering, pipe is pressed 40kV, electric current 30mA, 0.02 °/s of step-length, sweep limit: 5 °～70 °), Quanta200 type X ray energy dispersion spectrometer is to embodiment 1 step 1) Zn[B for preparing 3o 3(OH) 5] H 2o:Eu 3+with step 2) ZnB for preparing 2o 4: Eu 3+znB prepared by luminescent material and comparative example 1 2o 4: Eu 3+luminescent material characterizes, and the results are shown in Figure 1～6.
From Fig. 1,2a, 2b, Zn[B prepared by embodiment 1 3o 3(OH) 5] H 2o:Eu 3+, ZnB 2o 4: Eu 3+znB prepared by luminescent material and comparative example 1 2o 4: Eu 3+luminescent material all contains Zn, B, O and Eu element, illustrates that Eu successfully adulterates.
As seen from Figure 3, embodiment 1 step 1) diffraction data and the Zn[B of the product prepared 3o 3(OH) 5] H 2the diffraction data of the JCPDS standard card (File No.72-1789) of O is consistent, and can point out this product is Zn[B 3o 3(OH) 5] H 2o:Eu 3+.
From Fig. 4 a and Fig. 4 b, the diffraction data of luminescent material prepared by the luminescent material that embodiment 1 finally obtains and comparative example 1 all and ZnB 2o 4the diffraction data of JCPDS standard card (File No.39-1126) consistent, can point out prepared luminescent material is ZnB 2o 4: Eu 3+.
The ZnB that adopts Quanta200 type scanning electronic microscope to prepare embodiment 1 2o 4: Eu 3+znB prepared by luminescent material and comparative example 1 2o 4: Eu 3+luminescent material carries out morphology characterization, the results are shown in Figure 5a and Fig. 5 b.Contrasted ZnB prepared by embodiment 1 from two figure 2o 4: Eu 3+znB prepared by luminescent material and comparative example 1 2o 4: Eu 3+luminescent material is compared, and particle diameter is little.
Detected result shows, the ZnB that preparation method of the present invention obtains 2o 4: Eu 3+luminescent material particle diameter is 1 micron, and the variation up and down of particle diameter, in 0.05 micron, has demonstrated fabulous homogeneity; The ZnB that traditional preparation method of comparative example 1 obtains 2o 4: Eu 3+not etc., rangeability is very not large, is distributed between 1 micron to 20 microns for luminescent material size, and 15 microns of average out to, show that preparation method of the present invention has significantly reduced the particle diameter of final product.
Adopt F-4600 type spectrophotofluorometer (exciting slit width and transmitting slit width is all that 0.25nm. excitation wavelength is λ ex=260nm) to measure respectively ZnB prepared by embodiment 1 2o 4: Eu 3+znB prepared by luminescent material and comparative example 1 2o 4: Eu 3+luminescent material emmission spectrum at room temperature, the results are shown in Figure 6.
As can be seen from the figure, be 589,600,616 and 650nm place at wavelength, ZnB prepared by embodiment 1 2o 4: Eu 3+the luminous intensity of luminescent material is all obviously better than ZnB prepared by comparative example 1 2o 4: Eu 3+luminescent material, ZnB prepared by embodiment 1 2o 4: Eu 3+luminescent material wavelength be 589 and the luminous intensity at 600nm place be respectively 3042au and 1560au.
The above results shows, ZnB prepared by the inventive method 2o 4: Eu 3+znB prepared by luminescent material and conventional high-temperature solid phase method 2o 4: Eu 3+luminescent material is compared, and good dispersity and luminous intensity obviously improve.
Embodiment 2
At the preparation Zn[B of embodiment 1 3o 3(OH) 5] H 2o:Eu 3+in step 1, by 2.87g ZnSO 47H 2o, 1.91gNa 2b 4o 710H 2o and 0.05g Eu 2o 3be dissolved in 45mL distilled water ZnSO 47H 2o and Na 2b 4o 710H 2o, Eu 2o 3, redistilled water mol ratio be 1: 0.5: 0.03: 250, stirring at room temperature 36 hours, separates reaction product suction filtration, respectively with the each washing of redistilled water and dehydrated alcohol 3 times, be placed in baking oven 40 DEG C dry 24 hours, obtain Zn[B 3o 3(OH) 5] H 2o:Eu 3+.Other steps are identical with embodiment 1, are prepared into ZnB 2o 4: Eu 3+luminescent material.
Embodiment 3
At the preparation Zn[B of embodiment 1 3o 3(OH) 5] H 2o:Eu 3+in step 1, by 2.87g ZnSO 47H 2o, 5.72gNa 2b 4o 710H 2o and 0.07g Eu 2o 3be dissolved in 63mL distilled water ZnSO 47H 2o and Na 2b 4o 710H 2o, Eu 2o 3, redistilled water mol ratio be 1: 1.5: 0.04: 350, stirring at room temperature 14 hours, separates reaction product suction filtration, respectively with the each washing of redistilled water and dehydrated alcohol 3 times, be placed in baking oven 40 DEG C dry 24 hours, obtain Zn[B 3o 3(OH) 5] H 2o:Eu 3+.Other steps are identical with embodiment 1, are prepared into ZnB 2o 4: Eu 3+luminescent material.
Embodiment 4
At the preparation Zn[B of embodiment 1 3o 3(OH) 5] H 2o:Eu 3+in step 1, by 2.87g ZnSO 47H 2o, 11.43gNa 2b 4o 710H 2o and 1.05g Eu 2o 3be dissolved in 54mL distilled water ZnSO 47H 2o and Na 2b 4o 710H 2o, Eu 2o 3, redistilled water mol ratio be 1: 3: 0.1: 300, stirring at room temperature 48 hours, separates reaction product suction filtration, respectively with the each washing of redistilled water and dehydrated alcohol 3 times, be placed in baking oven 40 DEG C dry 24 hours, obtain Zn[B 3o 3(OH) 5] H 2o:Eu 3+.Other steps are identical with embodiment 1, are prepared into ZnB 2o 4: Eu 3+luminescent material.
Embodiment 5
At the preparation Zn[B of embodiment 1 3o 3(OH) 5] H 2o:Eu 3+in step 1, by 2.87g ZnSO 47H 2o, 3.81gNa 2b 4o 710H 2o and 0.01g Eu 2o 3be dissolved in 54mL distilled water ZnSO 47H 2o and Na 2b 4o 710H 2o, Eu 2o 3, redistilled water mol ratio be 1: 1: 0.01: 300, stirring at room temperature 72 hours, separates reaction product suction filtration, respectively with the each washing of redistilled water and dehydrated alcohol 3 times, be placed in baking oven 40 DEG C dry 24 hours, obtain Zn[B 3o 3(OH) 5] H 2o:Eu 3+.Other steps are identical with embodiment 1, are prepared into ZnB 2o 4: Eu 3+luminescent material.
Embodiment 6
At the preparation ZnB of embodiment 1 2o 4: Eu 3+in luminescent material step 2, the Zn[B that step 1 is obtained 3o 3(OH) 5] H 2o:Eu 3+800 DEG C of roastings 9 hours, other steps were identical with embodiment 1, obtain ZnB 2o 4: Eu 3+luminescent material, its wavelength be 589 and the luminous intensity at 599nm place be respectively 1946au and 994au.
Embodiment 7
At the preparation ZnB of embodiment 1 2o 4: Eu 3+in luminescent material step 2, the Zn[B that step 1 is obtained 3o 3(OH) 5] H 2o:Eu 3+800 DEG C of roastings 3 hours, other steps were identical with embodiment 1, obtain ZnB 2o 4: Eu 3+luminescent material, its wavelength be 589 and the luminous intensity at 600nm place be respectively 917au and 507au.
Embodiment 8
At the preparation ZnB of embodiment 1 2o 4: Eu 3+in luminescent material step 2, the Zn[B that step 1 is obtained 3o 3(OH) 5] H 2o:Eu 3+800 DEG C of roastings 6 hours, other steps were identical with embodiment 1, obtain ZnB 2o 4: Eu 3+luminescent material, its wavelength be 589 and the luminous intensity at 600nm place be respectively 2308au and 1285au.
Embodiment 9
At the preparation ZnB of embodiment 1 2o 4: Eu 3+in luminescent material step 2, the Zn[B that step 1 is obtained 3o 3(OH) 5] H 2o:Eu 3+900 DEG C of roastings 3 hours, other steps were identical with embodiment 1, obtain ZnB 2o 4: Eu 3+luminescent material, its wavelength be 589 and the luminous intensity at 600nm place be respectively 2795au and 1503au.
Embodiment 10
At the preparation ZnB of embodiment 1 2o 4: Eu 3+in luminescent material step 2, the Zn[B that step 1 is obtained 3o 3(OH) 5] H 2o:Eu 3+900 DEG C of roastings 9 hours, other steps were identical with embodiment 1, obtain ZnB 2o 4: Eu 3+luminescent material, its wavelength be 588 and the luminous intensity at 615nm place be respectively 2884au and 1540au.

Claims (10)

1.ZnB 2o 4: Eu 3+the preparation method of luminescent material, is characterized in that comprising the steps: 1) with ZnSO 47H 2o, Na 2b 4o 710H 2o and Eu 2o 3mix one-step synthesis and obtain Zn[B for raw material is added to the water 3o 3(OH) 5] H 2o:Eu 3+; 2) by gained Zn[B 3o 3(OH) 5] H 2o:Eu 3+at high temperature roasting inversion of phases obtains ZnB 2o 4: Eu 3+luminescent material.
2. according to the preparation method of claim 1, it is characterized in that step 1) ZnSO used 47H 2o, Na 2b 4o 710H 2o, Eu 2o 3, water mol ratio be 1: 0.5～3: 0.01～0.10: 250～550, reaction conditions is stirring reaction 12～72 hours under room temperature.
3. according to the preparation method of claim 2, it is characterized in that in room temperature reaction process, continuing to stir.
4. according to the preparation method of claim 2, characterized by further comprising reaction product suction filtration, washing, dry step.
5. according to the preparation method of claim 2, it is characterized in that ZnSO 47H 2o, Na 2b 4o 710H 2o, Eu 2o 3, water mol ratio be 1: 0.5～1.5: 0.03～0.08: 250～550, reaction conditions is stirring reaction 24～72 hours under room temperature.
6. according to the preparation method of claim 2, it is characterized in that ZnSO 47H 2o, Na 2b 4o 710H 2o, Eu 2o 3, water mol ratio be 1: 1: 0.06: 450, under room temperature, react 48 hours.
7. according to the preparation method of claim 1, it is characterized in that step 2) then cooling 700～1000 DEG C of roastings 3～9 hours.
8. according to the preparation method of claim 7, it is characterized in that step 2) then cooling 800～1000 DEG C of roastings 3～9 hours.
9. according to the preparation method of claim 7, it is characterized in that step 2) then cooling 900 DEG C of roastings 6 hours.
10. according to the preparation method of claim 1, it is characterized in that gained ZnB 2o 4: Eu 3+the median size of luminescent material is 1 micron.
CN201410249971.XA 2014-06-06 2014-06-06 The preparation method of ZnB2O4:Eu3+ luminescent material Expired - Fee Related CN104073252B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104845617A (en) * 2015-04-30 2015-08-19 陕西师范大学 Simple preparation method of Zn4B6O13: Eu3 + luminescent material
CN105018079A (en) * 2015-07-17 2015-11-04 辽宁大学 Preparation method of rare earth element-doped 4ZnO.B2O3.H2O: RE<3+>-type zinc borate
CN107235496A (en) * 2017-07-07 2017-10-10 辽宁大学 A kind of Firebrake ZB ZnB2O4The low temperature preparation method of luminescent material

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
ZHONGFEI MU ET.AL.: "《Enhanced red emission in ZnB2O4:Eu3+ by charge compensation》", 《OPTICAL MATERIALS》, 31 December 2011 (2011-12-31), pages 89 - 94 *
孙彦彬等: "《稀土发光材料的合成方法》", 《稀土》, vol. 24, no. 1, 31 December 2003 (2003-12-31), pages 43 - 48 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104845617A (en) * 2015-04-30 2015-08-19 陕西师范大学 Simple preparation method of Zn4B6O13: Eu3 + luminescent material
CN105018079A (en) * 2015-07-17 2015-11-04 辽宁大学 Preparation method of rare earth element-doped 4ZnO.B2O3.H2O: RE<3+>-type zinc borate
CN107235496A (en) * 2017-07-07 2017-10-10 辽宁大学 A kind of Firebrake ZB ZnB2O4The low temperature preparation method of luminescent material

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