CN105018079A - Preparation method of rare earth element-doped 4ZnO.B2O3.H2O: RE<3+>-type zinc borate - Google Patents

Preparation method of rare earth element-doped 4ZnO.B2O3.H2O: RE<3+>-type zinc borate Download PDF

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CN105018079A
CN105018079A CN201510426748.2A CN201510426748A CN105018079A CN 105018079 A CN105018079 A CN 105018079A CN 201510426748 A CN201510426748 A CN 201510426748A CN 105018079 A CN105018079 A CN 105018079A
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rare
doped
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4znob
zinc borate
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张向东
侯玉芳
葛春华
焦阳
佟建
关宏宇
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Liaoning University
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Liaoning University
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Abstract

The invention discloses a preparation method of rare earth element-doped 4ZnO.B2O3.H2O: RE<3+>-type zinc borate and belongs to the field of inorganic materials. The preparation method utilizes a direct hydro-thermal one step method to mix rare earth elements, a boron source and a zinc source. The preparation method can simply prepare zinc borate fluorescent powder with good luminescence performances. The product is a fluorescent material with good luminescence intensity and monochromaticity.

Description

A kind of 4ZnOB of doped with rare-earth elements 2o 3h 2o:RE 3+the preparation method of type zinc borate
Technical field
The invention belongs to field of inorganic materials, be specifically related to a kind of preparation method of 411 type zinc borates of doped with rare-earth elements, obtain a kind of inorganic fluorescent material with good luminous performance.
Background technology
Luminescent material great majority are solid inorganic materials, and it in parent lattice, at high temperature mixes the ion of another kind of element or atom and creates impurity defect thus luminous.China is the country that global rare earth resource is the abundantest.In the periodic table of elements, 15 lanthanon add scandium and yttrium totally 17 rare earth elements, and the luminescent material be made up of them is generally referred to as rare earth luminescent material.
The light sources of rare earth ion is in the transition of electron of the 4f shell do not filled up, because the electronics of 4f layer is shielded by 8 electron institutes of 5s and 5p electronic shell, crystal field is less on position of spectral line impact, and the energy level therefore in crystal field presents discrete level, and f-f transition emmission spectrum is line spectrum.
RE(rare earth) borate has the advantages such as highly stable physicochemical property, relatively low synthesis temperature and excellent luminescent properties, thus becomes the study hotspot of field of light emitting materials in recent years.Along with photoelectric technology to further develop with display equipment perfect, had a lot of RE(rare earth) borate to be taken as lamp phosphor and jumbotron flat-panel monitor fluorescent material.
Summary of the invention
The object of the invention is the preparation method of the 411 type zinc borates providing a kind of doped with rare-earth elements, and prepared the zinc borate inorganic fluorescent material with good luminous performance by comparatively easy method, products obtained therefrom luminous intensity is high, and monochromaticity is good.
The present invention for the adopted technical scheme that achieves the above object is: a kind of 4ZnOB of doped with rare-earth elements 2o 3h 2o:RE 3+the preparation method of type zinc borate, adopts Hydrothermal Synthesis single stage method, by rare earth element, boron source and the mixing of zinc source, obtains target product; Wherein, RE is rare earth element.
The 4ZnOB of above-mentioned a kind of doped with rare-earth elements 2o 3h 2o:RE 3+the preparation method of type zinc borate, be dissolved in respectively in deionized water in zinc source and boron source, rare earth element is dissolved in nitric acid, is mixed and is modulated into suspension liquid by three kinds of solution; Proceeded to by the suspension liquid of gained in airtight hydrothermal synthesis reaction still, carry out solvent thermal reaction 70-80 hour at 100-180 DEG C after, cooling, filters, and washing is dried.
The 4ZnOB of above-mentioned a kind of doped with rare-earth elements 2o 3h 2o:RE 3+the preparation method of type zinc borate, described zinc source is zinc sulfate or zinc nitrate.
The 4ZnOB of above-mentioned a kind of doped with rare-earth elements 2o 3h 2o:RE 3+the preparation method of type zinc borate, described boron source is boric acid or borax.
The 4ZnOB of above-mentioned a kind of doped with rare-earth elements 2o 3h 2o:RE 3+the preparation method of type zinc borate, described rare earth element is Eu 3+or Tb 3+.
The 4ZnOB of above-mentioned a kind of doped with rare-earth elements 2o 3h 2o:RE 3+the preparation method of type zinc borate, described rare earth element Eu 3+from europium nitrate or europium sesquioxide, and Eu 3+with Zn 2+mol ratio be 0.5% ~ 8.5%.
The 4ZnOB of above-mentioned a kind of doped with rare-earth elements 2o 3h 2o:RE 3+type zinc borate, described rare earth element tb 3+from Terbium trinitrate or terbium sesquioxide, and Tb 3+with Zn 2+mol ratio be 0.5% ~ 10.5%.
The 4ZnOB of the doped with rare-earth elements utilizing above-mentioned preparation method to prepare 2o 3h 2o:RE 3+type zinc borate uses as additive in luminescent material.
The invention has the beneficial effects as follows: the 4ZnOB of doped with rare-earth elements prepared by the present invention 2o 3h 2o:RE 3+type zinc borate, due to rare earth doped in zinc borate products, the monochromaticity of sample is good, can send good ruddiness or green glow.Present invention process is easy to control, simple to operate, preparation cycle is short, production cost is low, good product quality, can be obtained the doped with rare-earth elements 4ZnOB of different luminous intensity by control reaction conditions 2o 3h 2o zinc borate.
Accompanying drawing explanation
Fig. 1 is the 4ZnOB of the doped with rare-earth elements europium of the embodiment of the present invention 2 and 3 gained 2o 3h 2o:Eu 3+411 type zinc borate infrared spectrograms of doped with rare-earth elements are not had in type zinc borate and contrast experiment.
Wherein, 1, the comparative example of embodiment 14; 2, embodiment 2 product; 3, embodiment 3 product.
Fig. 2 is the 4ZnOB of the doped with rare-earth elements europium of the embodiment of the present invention 5 and 6 gained 2o 3h 2o:Eu 3+the scanning electron microscope (SEM) photograph of 411 type zinc borates of doped with rare-earth elements is not had in type zinc borate and contrast experiment.
Wherein, a: the comparative example of embodiment 14; B: embodiment 5 product; C: embodiment 6 product.
Fig. 3 is the 4ZnOB of the doped with rare-earth elements europium of the embodiment of the present invention 5 gained 2o 3h 2o:Eu 3+type zinc borate excitation spectrum.
Fig. 4 a is the X-ray powder diffraction of the comparative example of embodiment 14.
Fig. 4 b is the 4ZnOB of the doped with rare-earth elements terbium of the embodiment of the present invention 10 gained 2o 3h 2o:Tb 3+type zinc borate X-ray powder diffraction.
Fig. 5 is the 4ZnOB of the doped with rare-earth elements terbium of the embodiment of the present invention 12 gained 2o 3h 2o:Tb 3+type zinc borate emmission spectrum.
Embodiment
Below in conjunction with embodiment, the present invention is further described in detail, but is not limited to this.The pharmaceutical chemicals adopted in the following example is all commercial chemicals.
The 4ZnOB of embodiment 1 one kinds of doped with rare-earth elements europiums 2o 3h 2o:Eu 3+the preparation method of type zinc borate
Method is as follows:
1) take 0.5626g zinc sulfate to be dissolved in 3.0mL deionized water.
2) take 0.4084g boric acid and be dissolved in 5.0mL deionized water.
3) take 0.0018g europium sesquioxide to be dissolved in 2.0mL nitric acid.Eu 3+with Zn 2+mol ratio be 0.5%.
4) above-mentioned three kinds of solution are mixed and are modulated into suspension liquid.Gained suspension liquid is transferred in airtight hydrothermal synthesis reaction still, in 100 DEG C of reactions 72 hours, takes out reactor and be cooled to room temperature, filter out reaction product, washing, dry, obtain the 4ZnOB of doped with rare-earth elements europium 2o 3h 2o:Eu 3+type zinc borate.
The tristimulus coordinates calculated according to emmission spectrum is (0.6483,0.2514), and gained compound is the red fluorescence powder that monochromaticity is good.
The 4ZnOB of embodiment 2 one kinds of doped with rare-earth elements europiums 2o 3h 2o:Eu 3+the preparation method of type zinc borate
Method is as follows:
1) take 0.5541g zinc sulfate to be dissolved in 3.0mL deionized water.
2) take 0.4083g boric acid and be dissolved in 5.0mL deionized water.
3) take 0.0084g europium sesquioxide to be dissolved in 2.0mL nitric acid.Eu 3+with Zn 2+mol ratio be 2.5%.
4) above-mentioned three kinds of solution are mixed and are modulated into suspension liquid.Gained suspension liquid is transferred in airtight hydrothermal synthesis reaction still, in 150 DEG C of reactions 72 hours, takes out reactor and be cooled to room temperature, filter out reaction product, washing, dry, obtain the 4ZnOB of doped with rare-earth elements europium 2o 3h 2o:Eu 3+type zinc borate.
The tristimulus coordinates calculated according to emmission spectrum is (0.6448,0.3549), and gained compound is the red fluorescence powder that monochromaticity is good.
The 4ZnOB of embodiment 3 one kinds of doped with rare-earth elements europiums 2o 3h 2o:Eu 3+the preparation method of type zinc borate
Method is as follows:
1) take 0.5469g zinc nitrate to be dissolved in 3.0mL deionized water.
2) take 0.4083g boric acid and be dissolved in 5.0mL deionized water.
3) take 0.0120g europium nitrate to be dissolved in 2.0mL deionized water.Eu 3+with Zn 2+mol ratio be 4.5%.
4) above-mentioned three kinds of solution are mixed and are modulated into suspension liquid.Gained suspension liquid is transferred in airtight hydrothermal synthesis reaction still, in 180 DEG C of reactions 72 hours, takes out reactor and be cooled to room temperature, filter out reaction product, washing, dry, obtain the 4ZnOB of doped with rare-earth elements europium 2o 3h 2o:Eu 3+type zinc borate.
The tristimulus coordinates calculated according to emmission spectrum is (0.6449,0.3548), and gained compound is the red fluorescence powder that monochromaticity is good.
The 4ZnOB of embodiment 4 one kinds of doped with rare-earth elements europiums 2o 3h 2o:Eu 3+the preparation method of type zinc borate
Method is as follows:
1) take 0.5240g zinc nitrate to be dissolved in 3.0mL deionized water.
2) take 0.4087g boric acid and be dissolved in 5.0mL deionized water.
3) take 0.0206g europium sesquioxide to be dissolved in 2.0mL nitric acid.Eu 3+with Zn 2+mol ratio be 6.5%.
4) above-mentioned three kinds of solution are mixed and are modulated into suspension liquid.Gained suspension liquid is transferred in airtight hydrothermal synthesis reaction still, in 180 DEG C of reactions 72 hours, takes out reactor and be cooled to room temperature, filter out reaction product, washing, dry, obtain the 4ZnOB of doped with rare-earth elements europium 2o 3h 2o:Eu 3+type zinc borate.
The tristimulus coordinates calculated according to emmission spectrum is (0.6464,0.3533), and gained compound monochromaticity is good, the red fluorescence powder that luminous intensity is good.
The 4ZnOB of embodiment 5 one kinds of doped with rare-earth elements europiums 2o 3h 2o:Eu 3+the preparation method of type zinc borate
Method is as follows:
1) take 0.5178g zinc nitrate to be dissolved in 3.0mL deionized water.
2) take 0.4084g boric acid and be dissolved in 5.0mL deionized water.
3) take 0.0235g europium sesquioxide to be dissolved in 2.0mL nitric acid.Eu 3+with Zn 2+mol ratio be 7.5%.
4) above-mentioned three kinds of solution are mixed and are modulated into suspension liquid.Gained suspension liquid is transferred in airtight hydrothermal synthesis reaction still, in 180 DEG C of reactions 72 hours, takes out reactor and be cooled to room temperature, filter out reaction product, washing, dry, obtain the 4ZnOB of doped with rare-earth elements europium 2o 3h 2o:Eu 3+type zinc borate.
The tristimulus coordinates calculated according to emmission spectrum is (0.6455,0.3542), and gained compound is that monochromaticity is good, the red fluorescence powder that luminous intensity is good.
The 4ZnOB of embodiment 6 one kinds of doped with rare-earth elements europiums 2o 3h 2o:Eu 3+the preparation method of type zinc borate
Method is as follows:
1) take 0.5105g zinc nitrate to be dissolved in 3.0mL deionized water.
2) take 0.4083g boric acid and be dissolved in 5.0mL deionized water.
3) take 0.0264g europium nitrate to be dissolved in 2.0mL deionized water.Eu 3+with Zn 2+mol ratio be 8.5%.
4) above-mentioned three kinds of solution are mixed and are modulated into suspension liquid.Gained suspension liquid is transferred in airtight hydrothermal synthesis reaction still, in 180 DEG C of reactions 72 hours, takes out reactor and be cooled to room temperature, filter out reaction product, washing, dry, obtain the 4ZnOB of doped with rare-earth elements europium 2o 3h 2o:Eu 3+type zinc borate.
The tristimulus coordinates calculated according to emmission spectrum is (0.6426,0.3542), and gained compound is that monochromaticity is good, the red fluorescence powder that luminous intensity is good.
The 4ZnOB of embodiment 7 one kinds of doped with rare-earth elements terbiums 2o 3h 2o:Tb 3+the preparation method of type zinc borate
Method is as follows:
1) take 0.5459g zinc sulfate to be dissolved in 3.0mL deionized water.
2) take 0.4078g borax and be dissolved in 5.0mL deionized water.
3) take 0.0019g terbium sesquioxide to be dissolved in 2.0mL nitric acid.Tb 3+with Zn 2+mol ratio be 0.5%.
4) above-mentioned three kinds of solution are mixed and are modulated into suspension liquid.Gained suspension liquid is transferred in airtight hydrothermal synthesis reaction still, in 100 DEG C of reactions 72 hours, takes out reactor and be cooled to room temperature, filter out reaction product, washing, dry, obtain the 4ZnOB of doped with rare-earth elements terbium 2o 3h 2o:Tb 3+type zinc borate.
The tristimulus coordinates calculated according to emmission spectrum is (0.2598,0.5313), illustrates that this compound can send green glow and monochromaticity is good
The 4ZnOB of embodiment 8 one kinds of doped with rare-earth elements terbiums 2o 3h 2o:Tb 3+the preparation method of type zinc borate
Method is as follows:
1) take 0.5382g zinc nitrate to be dissolved in 3.0mL deionized water.
2) take 0.4084g borax and be dissolved in 5.0mL deionized water.
3) take 0.090g terbium sesquioxide to be dissolved in 2.0mL nitric acid.Tb 3+with Zn 2+mol ratio be 2.5%.
4) above-mentioned three kinds of solution are mixed and are modulated into suspension liquid.Gained suspension liquid is transferred in airtight hydrothermal synthesis reaction still, in 100 DEG C of reactions 72 hours, takes out reactor and be cooled to room temperature, filter out reaction product, washing, dry, obtain the 4ZnOB of doped with rare-earth elements terbium 2o 3h 2o:Tb 3+type zinc borate.
The tristimulus coordinates calculated according to emmission spectrum is (0.2725,0.5519), illustrates that this compound can send green glow and monochromaticity is good
The 4ZnOB of embodiment 9 one kinds of doped with rare-earth elements terbiums 2o 3h 2o:Tb 3+the preparation method of type zinc borate
Method is as follows:
1) take 0.5380g zinc nitrate to be dissolved in 3.0mL deionized water.
2) take 0.4083g boric acid and be dissolved in 5.0mL deionized water.
3) take 0.0161g Terbium trinitrate to be dissolved in 2.0mL deionized water.Tb 3+with Zn 2+mol ratio be 4.5%.
4) above-mentioned three kinds of solution are mixed and are modulated into suspension liquid.Gained suspension liquid is transferred in airtight hydrothermal synthesis reaction still, in 140 DEG C of reactions 72 hours, takes out reactor and be cooled to room temperature, filter out reaction product, washing, dry, obtain the 4ZnOB of doped with rare-earth elements terbium 2o 3h 2o:Tb 3+type zinc borate.
The tristimulus coordinates calculated according to emmission spectrum is (0.2732,0.5515), illustrates that this compound can send green glow and monochromaticity is good.
The 4ZnOB of embodiment 10 1 kinds of doped with rare-earth elements terbiums 2o 3h 2o:Tb 3+the preparation method of type zinc borate
Method is as follows:
1) take 0.5314g zinc nitrate to be dissolved in 3.0mL deionized water.
2) take 0.4083g boric acid and be dissolved in 5.0mL deionized water.
3) take 0.0190g Terbium trinitrate to be dissolved in 2.0mL deionized water.Tb 3+with Zn 2+mol ratio be 5.5%.
Above-mentioned three kinds of solution are mixed and are modulated into suspension liquid.Gained suspension liquid is transferred in airtight hydrothermal synthesis reaction still, in 140 DEG C of reactions 72 hours, takes out reactor and be cooled to room temperature, filter out reaction product, washing, dry, obtain the 4ZnOB of doped with rare-earth elements terbium 2o 3h 2o:Tb 3+type zinc borate.
The tristimulus coordinates calculated according to emmission spectrum is (0.2732,0.5515), illustrates that this compound can send green glow and monochromaticity is good.
The 4ZnOB of embodiment 11 1 kinds of doped with rare-earth elements terbiums 2o 3h 2o:Tb 3+the preparation method of type zinc borate
Method is as follows:
1) take 0.5169g zinc sulfate to be dissolved in 3.0mL deionized water.
2) take 0.4081g boric acid and be dissolved in 5.0mL deionized water.
3) take 0.0252g terbium sesquioxide to be dissolved in 2.0mL nitric acid.Tb 3+with Zn 2+mol ratio be 7.5%.
4) above-mentioned three kinds of solution are mixed and are modulated into suspension liquid.Gained suspension liquid is transferred in airtight hydrothermal synthesis reaction still, in 180 DEG C of reactions 72 hours, takes out reactor and be cooled to room temperature, filter out reaction product, washing, dry, obtain the 4ZnOB of doped with rare-earth elements terbium 2o 3h 2o:Tb 3+type zinc borate.
The tristimulus coordinates calculated according to emmission spectrum is (0.2732,0.5515), illustrates that this compound can send green glow and monochromaticity is good.
The 4ZnOB of embodiment 12 1 kinds of doped with rare-earth elements terbiums 2o 3h 2o:Tb 3+the preparation method of type zinc borate
Method is as follows:
1) take 0.5112g zinc nitrate to be dissolved in 3.0mL deionized water.
2) take 0.4077g boric acid and be dissolved in 5.0mL deionized water.
3) take 0.0283g terbium sesquioxide to be dissolved in 2.0mL nitric acid.Tb 3+with Zn 2+mol ratio be 8.5%.
4) above-mentioned three kinds of solution are mixed and are modulated into suspension liquid.Gained suspension liquid is transferred in airtight hydrothermal synthesis reaction still, in 180 DEG C of reactions 72 hours, takes out reactor and be cooled to room temperature, filter out reaction product, washing, dry, obtain the 4ZnOB of doped with rare-earth elements terbium 2o 3h 2o:Tb 3+type zinc borate.
The tristimulus coordinates calculated according to emmission spectrum is (0.2813,0.5613), illustrates that this compound can send green glow and monochromaticity is good.
The 4ZnOB of embodiment 13 1 kinds of doped with rare-earth elements terbiums 2o 3h 2o:Tb 3+the preparation method of type zinc borate
Method is as follows:
1) take 0.5033g zinc sulfate to be dissolved in 3.0mL deionized water.
2) take 0.4087g boric acid and be dissolved in 5.0mL deionized water.
3) take 0.0312g terbium sesquioxide to be dissolved in 2.0mL nitric acid.Tb 3+with Zn 2+mol ratio be 9.5%.
4) above-mentioned three kinds of solution are mixed and are modulated into suspension liquid.Gained suspension liquid is transferred in airtight hydrothermal synthesis reaction still, in 180 DEG C of reactions 72 hours, takes out reactor and be cooled to room temperature, filter out reaction product, washing, dry, obtain the 4ZnOB of doped with rare-earth elements terbium 2o 3h 2o:Tb 3+type zinc borate.
The tristimulus coordinates calculated according to emmission spectrum is (0.2565,0.5274), illustrates that this compound can send green glow and monochromaticity is good.
Embodiment 14 contrasts case
1) take 0.5239g zinc sulfate to be dissolved in 3.0mL deionized water.
2) take 0.4084g boric acid to be dissolved in 5.0mL deionized water.
3) the two mixed and be modulated into suspension liquid.Be transferred to by gained solution in 180 DEG C of reactions 72 hours in airtight hydrothermal synthesis reaction still, take out reactor and be cooled to room temperature, filter out reaction product, washing, dries to obtain 4ZnOB 2o 3h 2o type zinc borate.
As seen from Figure 1, to the Eu that do not adulterate 3+the charateristic avsorption band of zinc borate compound belong to: 3360 and 3367cm -1absorption band belong to O-H stretching vibration; 1350 and 1310cm -1the peak at place belongs to the symmetry of B – O and asymmetric stretching vibration; 1250cm -1peak belong to the in-plane bending vibration of B-O-H; 717cm -1peak belong to the out-of-plane deformation vibration of B – O; Sample 2 and 3 is different concns Eu 3+the infrared spectrum of the zinc borate compound of doping, its infrared charateristic avsorption band and the Eu that do not adulterate 3+zinc borate compound contrast substantially without change, Eu is described 3+when shared concentration is less, the impact caused final product structure is little.
As seen from Figure 2, do not adulterate Eu 3+the club shaped structure that the pattern of the compound a of ion is differed by thickness forms, and large has 2-3 μm wide, and little can reach nano level.Along with Eu 3+the increase of doping content, the pattern of sample there occurs change.Work as Eu 3+ion mixes 4ZnOB 2o 3h 2o, there is agglomeration in club shaped structure, trends towards generating flower-like structure, and sample topography gradually becomes mixed structure.
Fig. 3 is the emmission spectrum of the compound 5 under the monitoring of 253nm excitation wavelength, and wavelength region is 550-750nm.In figure, the emission peak of compound is from Eu 3+excited state 5d 0energy level is to ground state 7f jthe transition of (J=0,1,2,3,4) energy level.578,592,614,653 and the emission peak at 701nm place correspond respectively to Eu 3+ion 5d 07f j(J=0 ~ 4) transition.The strongest emission peak is 615nm place 5d 07f 2electric dipole transition, can send good ruddiness.
Fig. 4 b is the XRD spectra of compound 10.With the Eu that do not adulterate 3+the spectrogram of zinc borate (Fig. 4 a) is consistent, and without considerable change, shows a small amount of Tb 3+after ion adds, the product obtained also still has 411 type zinc borate structures, Tb 3+ion is successfully doped in the host lattice of zinc borate, and a small amount of Tb 3+doping does not cause obvious lattice variations yet.
Fig. 5 is the emmission spectrum of the compound 12 under the monitoring of 236nm excitation wavelength, and wavelength region is 450-650nm.In the drawings, the emission peak of the emmission spectrum of compound is from Tb 3+excited state 5d 4energy level is to ground state 7f jthe transition of (J=6,5,4,3).489,544,583 and the emission peak at 622nm place correspond respectively to 5d 47f 6, 5d 47f 5, 5d 47f 4with 5d 47f 3transition.Sample luminous intensity highest peak shown in figure for 545nm place 5d 47f 5transition, illustrates that compound can launch good green glow.

Claims (10)

1. the 4ZnOB of a doped with rare-earth elements 2o 3h 2o:RE 3+the preparation method of type zinc borate, is characterized in that: adopt Hydrothermal Synthesis single stage method, by rare earth element, boron source and the mixing of zinc source, obtains target product; Wherein, RE is rare earth element.
2. the 4ZnOB of a kind of doped with rare-earth elements according to claim 1 2o 3h 2o:RE 3+the preparation method of type zinc borate, is characterized in that: be dissolved in respectively in deionized water in zinc source and boron source, rare earth element is dissolved in nitric acid, is mixed and is modulated into suspension liquid by three kinds of solution; Proceeded to by the suspension liquid of gained in airtight hydrothermal synthesis reaction still, carry out solvent thermal reaction 70-80 hour at 100-180 DEG C after, cooling, filters, and washing is dried.
3. the 4ZnOB of a kind of doped with rare-earth elements according to claim 1 and 2 2o 3h 2o:RE 3+the preparation method of type zinc borate, is characterized in that: described zinc source is zinc sulfate or zinc nitrate.
4. the 4ZnOB of a kind of doped with rare-earth elements according to claim 1 and 2 2o 3h 2o:RE 3+the preparation method of type zinc borate, is characterized in that: described boron source is boric acid or borax.
5. the 4ZnOB of a kind of doped with rare-earth elements according to claim 1 and 2 2o 3h 2o:RE 3+the preparation method of type zinc borate, is characterized in that: described rare earth elements RE 3+for Eu 3+or Tb 3+.
6. the 4ZnOB of a kind of doped with rare-earth elements according to claim 5 2o 3h 2o:RE 3+the preparation method of type zinc borate, is characterized in that: described rare earth element Eu 3+from europium nitrate or europium sesquioxide.
7. the 4ZnOB of a kind of doped with rare-earth elements according to claim 6 2o 3h 2o:RE 3+the preparation method of type zinc borate, is characterized in that: Eu 3+with Zn 2+mol ratio be 0.5% ~ 8.5%.
8. the 4ZnOB of a kind of doped with rare-earth elements according to claim 5 2o 3h 2o:RE 3+the preparation method of type zinc borate, is characterized in that: described rare earth element tb 3+from Terbium trinitrate or terbium sesquioxide.
9. the 4ZnOB of a kind of doped with rare-earth elements according to claim 8 2o 3h 2o:RE 3+the preparation method of type zinc borate, is characterized in that: Tb 3+with Zn 2+mol ratio be 0.5% ~ 10.5%.
10. the 4ZnOB of the doped with rare-earth elements utilizing the preparation method described in claim 1 or 2 to prepare 2o 3h 2o:RE 3+type zinc borate in luminescent material as the application of additive.
CN201510426748.2A 2015-07-17 2015-07-17 Preparation method of rare earth element-doped 4ZnO.B2O3.H2O: RE<3+>-type zinc borate Pending CN105018079A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109439319A (en) * 2018-12-28 2019-03-08 陕西师范大学 A kind of preparation method of treasure maesa herb globular nanostructures luminescent material

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000230111A (en) * 1999-02-09 2000-08-22 Sumitomo Bakelite Co Ltd Epoxy resin composition and semiconductor device
CN101676361A (en) * 2008-09-16 2010-03-24 中国科学院福建物质结构研究所 Europium-ion-doped barium molybdate nano luminescent powder and preparation method thereof
CN101704532A (en) * 2009-11-10 2010-05-12 武汉大学 Preparation method of zinc borate
CN103275707A (en) * 2013-05-28 2013-09-04 陕西师范大学 Preparation method of CaB2O4: Eu<3+> luminescent material
CN103525417A (en) * 2013-09-23 2014-01-22 武汉理工大学 Preparation method of europium-doped hydroxyapatite (HAP) fluorescent nanoparticles
CN104073252A (en) * 2014-06-06 2014-10-01 陕西师范大学 Preparation method of ZnB2O4:Eu<3+> luminescent material
CN104592991A (en) * 2015-01-26 2015-05-06 陕西师范大学 Spherical Zn6O(OH)(BO3)3: Eu<3+> luminescent material and preparation method thereof
CN104610965A (en) * 2015-01-09 2015-05-13 南昌大学 Preparation method of spherical fluorescent powder

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000230111A (en) * 1999-02-09 2000-08-22 Sumitomo Bakelite Co Ltd Epoxy resin composition and semiconductor device
CN101676361A (en) * 2008-09-16 2010-03-24 中国科学院福建物质结构研究所 Europium-ion-doped barium molybdate nano luminescent powder and preparation method thereof
CN101704532A (en) * 2009-11-10 2010-05-12 武汉大学 Preparation method of zinc borate
CN103275707A (en) * 2013-05-28 2013-09-04 陕西师范大学 Preparation method of CaB2O4: Eu<3+> luminescent material
CN103525417A (en) * 2013-09-23 2014-01-22 武汉理工大学 Preparation method of europium-doped hydroxyapatite (HAP) fluorescent nanoparticles
CN104073252A (en) * 2014-06-06 2014-10-01 陕西师范大学 Preparation method of ZnB2O4:Eu<3+> luminescent material
CN104610965A (en) * 2015-01-09 2015-05-13 南昌大学 Preparation method of spherical fluorescent powder
CN104592991A (en) * 2015-01-26 2015-05-06 陕西师范大学 Spherical Zn6O(OH)(BO3)3: Eu<3+> luminescent material and preparation method thereof

Non-Patent Citations (6)

* Cited by examiner, † Cited by third party
Title
A. IVANKOV ET AL.,: ""Optical properties of Eu3+-doped zinc borate glasses"", 《JOURNAL OF LUMINESCENCE》 *
J. LIU ET AL.,: ""The effects of charge compensation on photoluminescence properties of a new green-emitting ZnB2O4:Tb3+ phosphor"", 《LUMINESCENCE》 *
Y. GAO ET AL.,: ""Hydrothermal Synthesis and Standard Molar Enthalpy of Formation of ZincBorate of 4ZnO·B2O3·H2O"", 《J. CHEM. ENG. DATA》 *
Y. ZHENG ET AL.,: ""Effect of Eu3+-doped on the luminescence properties of zinc borate nanoparticles"", 《COLLOIDS AND SURFACES A: PHYSICOCHEM. ENG. ASPECTS》 *
乐天等,: ""Eu3+掺杂2ZnO·2.2B2O3·3H2O 红色荧光粉的发光性能"", 《发光学报》 *
乐天等,: ""Tb3+ -Eu3+共掺杂2ZnO·2.2B2O3·3H2O的制备和发光性能"", 《人工晶体学报》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109439319A (en) * 2018-12-28 2019-03-08 陕西师范大学 A kind of preparation method of treasure maesa herb globular nanostructures luminescent material
CN109439319B (en) * 2018-12-28 2021-09-14 陕西师范大学 Preparation method of hollow flower ball-shaped nano-structure luminescent material

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