CN105694874A - Preparation method of polyhedral InBO3:Eu<3+> luminescent material - Google Patents
Preparation method of polyhedral InBO3:Eu<3+> luminescent material Download PDFInfo
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- CN105694874A CN105694874A CN201610187598.9A CN201610187598A CN105694874A CN 105694874 A CN105694874 A CN 105694874A CN 201610187598 A CN201610187598 A CN 201610187598A CN 105694874 A CN105694874 A CN 105694874A
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Abstract
The invention discloses a preparation method of a polyhedral InBO3:Eu<3+> luminescent material. The method comprises the following step: by using indium nitrate or indium oxide as an indium source and potassium tetraborate, sodium borate or anhydrous lithium borate as a boron source, directly carrying out one-step reaction to prepare the hexahedral, octahedral or any polyhedral InBO3:Eu<3+> luminescent material. The method is simple, and has the advantages of mild reaction conditions and accessible raw materials. The polyhedral InBO3:Eu<3+> luminescent material has the advantages of favorable dispersity, uniform shape and higher luminescent intensity, and is applicable to the fields of display and development, light sources, medicine and the like.
Description
Technical field
The invention belongs to luminescent material technical field, be specifically related to the polyhedral InBO that a kind of luminous intensity is high3:Eu3+The preparation method of luminescent material。
Background technology
Due to borate substrate luminescent material have simpler than with silicate, aluminate and phosphate for substrate luminescent material synthesis technique, stable chemical nature, color rendering properties are good, luminous efficiency high, this has been carried out substantial amounts of research by people in recent years, achieving certain progress in its luminescent properties, luminescence mechanism research etc., in the different field such as display development, light source, optoelectronics, medical science, oneself obtains and utilizes widely。
Common borate substrate has: rare-earth borate, alkaline earth metal borate, rare earth and alkaline-earth metal Composite borate and binary rare-earth metal perborate base status。At present, mainly utilizing the methods such as high temperature solid-state method, sol-gel process, combustion method to synthesize different types of borate substrate luminescent material, wherein high temperature solid-state method is to prepare these anhydrous borate substrate luminescent material most common methods。Such as, Shu Wangen et al. calcines at 1200 DEG C with high temperature solid-state method and has synthesized the InBO that a kind of luminous intensity is high3:Eu3+Fluorescent material (Central South University's Master's thesis: the preparation of boric acid indium fluorescent RE powder and the research of fluorescent characteristic thereof), its burn red, in the daylighting fields such as nowadays LED very promising, but the method needs long-time high-temperature calcination, and the chemical composition homogeneity of product is poor, broad particle distribution, appearance are irregular；Te-HuaFang et al. utilizes sol-gel process to prepare InBO3:Eu3+Fluorescent material (Int.J.Electrochem.Sci., 10 (2015) 2391-2399), although the method can overcome the shortcoming needing long-time high-temperature calcination that high temperature solid-state method exists, but gained fluorescent material pattern is single, particle diameter is less, is unfavorable for fluorescent emission；JyotsnaThakur etc. adopt combustion method to prepare InBO3:Eu3+Fluorescent material (J.Am.Ceram.Soc., 95 [2] 696-704 (2012)), the method preparation temperature is low, and be prepared in the way of solution, be conducive to fully reacting between material, but gained fluorescent material excitation is relatively low, is unfavorable for products application。Result of study shows, the performance of borate substrate luminescent material is had a great impact by pattern, for instance YanpingLi et al. utilizes hydro-thermal method to prepare the LuBO of different-shape3:Eu3+(Chem.Mater.2009,21,468-475), pattern is different, and its performance is also different。
Summary of the invention
The technical problem to be solved is in that to overcome existing InBO3:Eu3+The shortcoming that luminescent material preparation method exists, it is provided that a kind of simple to operate, reaction condition is gentle and products obtained therefrom morphology controllable, good dispersion, fluorescence is strong, excitation is high polyhedral InBO3:Eu3+The preparation method of luminescent material。
Solve the technical scheme that above-mentioned technical problem adopts: by indium source, boron source, Eu2O3And H2O is 1:2～10:0.01～0.10:80～310 mix homogeneously in molar ratio, gained mixture is transferred in the stainless steel autoclave of teflon lined, 180～240 DEG C are reacted 1～5 day, 2～3 times will be respectively washed with 60～80 DEG C of hot water, ethanol successively after product sucking filtration, 50～60 DEG C dry 12～24 hours, obtain polyhedral InBO3:Eu3+Luminescent material, wherein said indium source is indium nitrate or Indium sesquioxide., and described boron source is any one in dipotassium tetraborate, sodium tetraborate, anhydrous boric acid lithium。
The preferred indium source of the present invention, boron source, Eu2O3And H2The mol ratio of O is 1:3～8:0.03～0.09:100～230, it is preferred that indium source, boron source, Eu2O3And H2The mol ratio of O is 1:3～6:0.09:100。
The present invention reacts 2～3 days at 200～240 DEG C, and optimum selection is reacted 3 days at 220 DEG C。
When above-mentioned boron source is dipotassium tetraborate or sodium tetraborate, polyhedral InBO3:Eu3+Luminescent material is hexahedron shape。
When above-mentioned boron source is anhydrous boric acid lithium, polyhedral InBO3:Eu3+Luminescent material is octahedra shape。
The inventive method is simple, and raw material is easy to get, and reaction condition is gentle, prepared InBO3:Eu3+Luminescent material good dispersion, pattern is various, and excitation is high, and than InBO prepared by conventional high-temperature solid phase method3:Eu3+Luminescent material has higher luminous intensity, can be applicable to the different field such as display development, light source, medical science。
Accompanying drawing explanation
Fig. 1 is the hexahedron shape InBO of embodiment 1 preparation3:Eu3+The EDS figure of luminescent material。
Fig. 2 is the hexahedron shape InBO of embodiment 1 preparation3:Eu3+The XRD figure of luminescent material。
Fig. 3 is the hexahedron shape InBO of embodiment 1 preparation3:Eu3+The SEM figure of luminescent material。
Fig. 4 is the hexahedron shape InBO of embodiment 1 preparation3:Eu3+The PL figure of luminescent material。
Fig. 5 is the hexahedron shape InBO of embodiment 2 preparation3:Eu3+The SEM figure of luminescent material。
Fig. 6 is the hexahedron shape InBO of embodiment 3 preparation3:Eu3+The SEM figure of luminescent material。
Fig. 7 is the octahedra shape InBO of embodiment 4 preparation3:Eu3+The SEM figure of luminescent material。
Fig. 8 is the octahedra shape InBO of embodiment 5 preparation3:Eu3+The SEM figure of luminescent material。
Fig. 9 is the octahedra shape InBO of embodiment 6 preparation3:Eu3+The SEM figure of luminescent material。
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is described in more detail, but protection scope of the present invention is not limited only to these embodiments。
Embodiment 1
By 0.097g (0.35mmol) Indium sesquioxide., 0.32g (1.05mmol) dipotassium tetraborate, 0.0037g (0.0105mmol) Eu2O3、0.63mL(35mmol)H2O mix homogeneously, gained mixture is transferred in the stainless steel autoclave of teflon lined, and 220 DEG C are reacted 72 hours, will respectively wash 3 times with the hot water of 60～80 DEG C, ethanol successively after product sucking filtration, 60 DEG C of baking oven inner dryings 24 hours, obtain hexahedron shape InBO3:Eu3+Luminescent material。
(working condition is: Cu target Ka line to adopt RigakuD/MAX-IIIC type x-ray powder diffraction instrument, graphite flake filters, pipe pressure 40kV, electric current 30mA, 0.02 °/s of step-length, sweep limits: 10 °～70 °), Quanta200 type X-ray energy dispersion spectrum analyser, Quanta200 type scanning electron microscope, F-7000 type spectrofluorophotometer (excite slit width and launch slit width be all 0.5 and 0.5nm, voltage is 500V, excitation wavelength is λ ex=237nm) gained luminescent material is characterized, result is shown in Fig. 1～4。As seen from Figure 1, containing In, B, O and Eu element in gained luminescent material, illustrate that Eu successfully adulterates。From Figure 2 it can be seen that the diffraction data of gained luminescent material and InBO3The diffraction data of JCPDS standard card (FileNo.17-0933) consistent, occur without other impurity peaks, illustrate that the purity of luminescent material obtained is significantly high。As seen from Figure 3, gained InBO3:Eu3+Luminescent material is ganoid hexahedron pattern, good dispersion and uniform particle sizes。From fig. 4, it can be seen that gained InBO3:Eu3+Luminescent material is that 591nm, 598nm and 613nm place has obvious Eu at wavelength3+Characteristic peak, was InBO before 550nm3Substrate peak, wavelength be 591nm and 613nm place luminous intensity respectively 2843au and 299au。
Embodiment 2
By 0.097g (0.35mmol) Indium sesquioxide., 0.53g (1.4mmol) sodium tetraborate, 0.0037g (0.0105mmol) Eu2O3、1.95mL(108.5mmol)H2O mix homogeneously, gained mixture is transferred in the stainless steel autoclave of teflon lined, and 200 DEG C are reacted 60 hours, will respectively wash 3 times with the hot water of 60～80 DEG C, ethanol successively after product sucking filtration, 60 DEG C of baking oven inner dryings 24 hours, obtain hexahedron shape InBO3:Eu3+Luminescent material (see Fig. 5), it is at luminous intensity respectively 2840au and the 520au that wavelength is 591nm and 613nm place。
Embodiment 3
By 0.199g (0.66mmol) indium nitrate, 1g (2.64mmol) sodium tetraborate, 0.0186g (0.053mmol) Eu2O3、1.2mL(66mmol)H2O mix homogeneously, gained mixture is transferred in the stainless steel autoclave of teflon lined, and 240 DEG C are reacted 48 hours, will respectively wash 3 times with the hot water of 60～80 DEG C, ethanol successively after product sucking filtration, 60 DEG C of baking oven inner dryings 24 hours, obtain hexahedron shape InBO3:Eu3+Luminescent material (see Fig. 6), it is at luminous intensity respectively 1240au and the 350au that wavelength is 591nm and 613nm place。
Embodiment 4
By 0.0953g (0.34mmol) Indium sesquioxide., 0.35g (2.04mmol) anhydrous boric acid lithium, 0.0060g (0.017mmol) Eu2O3、0.70mL(39mmol)H2O mix homogeneously, gained mixture is transferred in the stainless steel autoclave of teflon lined, and 220 DEG C are reacted 72 hours, will respectively wash 3 times with the hot water of 60～80 DEG C, ethanol successively after product sucking filtration, 60 DEG C of baking oven inner dryings 24 hours, obtain octahedra shape InBO3:Eu3+Luminescent material (see Fig. 7), it is at luminous intensity respectively 2170au and the 485au that wavelength is 591nm and 613nm place。
Embodiment 5
By 0.208g (0.69mmol) nitrate, 0.7g (4.14mmol) anhydrous boric acid lithium, 0.0097g (0.0276mmol) Eu2O3、1mL(55mmol)H2O mix homogeneously, gained mixture is transferred in the stainless steel autoclave of teflon lined, and 240 DEG C are reacted 54 hours, will respectively wash 3 times with the hot water of 60～80 DEG C, ethanol successively after product sucking filtration, 60 DEG C of baking oven inner dryings 24 hours, obtain octahedra shape InBO3:Eu3+Luminescent material (see Fig. 8), it is at luminous intensity respectively 1500au and the 330au that wavelength is 591nm and 613nm place。
Embodiment 6
By 0.091g (0.33mmol) Indium sesquioxide., 0.53g (1.75mmol) dipotassium tetraborate, 0.0105g (0.03mmol) Eu2O3、1.5mL(80.5mmol)H2O mix homogeneously, gained mixture is transferred in the stainless steel autoclave of teflon lined, and 200 DEG C are reacted 54 hours, will respectively wash 3 times with the hot water of 60～80 DEG C, ethanol successively after product sucking filtration, 60 DEG C of baking oven inner dryings 24 hours, obtain octahedra shape InBO3:Eu3+Luminescent material (see Fig. 9), it is at luminous intensity respectively 1573au and the 270au that wavelength is 591nm and 613nm place。
Claims (7)
1. a polyhedral InBO3:Eu3+The preparation method of luminescent material, it is characterised in that: by indium source, boron source, Eu2O3And H2O is 1:2～10:0.01～0.10:80～310 mix homogeneously in molar ratio, gained mixture is transferred in the stainless steel autoclave of teflon lined, react 1～5 day at 180～240 DEG C, 2～3 times will be respectively washed with 60～80 DEG C of hot water, ethanol successively after product sucking filtration, 50～60 DEG C dry 12～24 hours, obtain polyhedral InBO3:Eu3+Luminescent material, wherein said indium source is indium nitrate or Indium sesquioxide., and described boron source is any one in dipotassium tetraborate, sodium tetraborate, anhydrous boric acid lithium。
2. polyhedral InBO according to claim 13:Eu3+The preparation method of luminescent material, it is characterised in that: described indium source, boron source, Eu2O3And H2The mol ratio of O is 1:3～8:0.03～0.09:100～230。
3. polyhedral InBO according to claim 13:Eu3+The preparation method of luminescent material, it is characterised in that: described indium source, boron source, Eu2O3And H2The mol ratio of O is 1:3～6:0.09:100。
4. the polyhedral InBO according to claims 1 to 3 any one3:Eu3+The preparation method of luminescent material, it is characterised in that: react 2～3 days at 200～240 DEG C。
5. the polyhedral InBO according to claims 1 to 3 any one3:Eu3+The preparation method of luminescent material, it is characterised in that: react 3 days at 220 DEG C。
6. polyhedral InBO according to claim 13:Eu3+The preparation method of luminescent material, it is characterised in that: when described boron source is dipotassium tetraborate or sodium tetraborate, polyhedral InBO3:Eu3+Luminescent material is hexahedron shape。
7. polyhedral InBO according to claim 13:Eu3+The preparation method of luminescent material, it is characterised in that: when described boron source is anhydrous boric acid lithium, polyhedral InBO3:Eu3+Luminescent material is octahedra shape。
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0159085A1 (en) * | 1984-04-12 | 1985-10-23 | Koninklijke Philips Electronics N.V. | Cathode-ray tube |
| CN85102041A (en) * | 1985-04-01 | 1986-10-29 | 菲利浦光灯制造公司 | Cathode ray tube |
| CN1643640A (en) * | 2002-03-28 | 2005-07-20 | 株式会社东芝 | X-ray image tube, x-ray image tube device and x-ray device |
| CN1974885A (en) * | 2006-11-16 | 2007-06-06 | 同济大学 | Low temperature process of preparing RE borate crystal with oxide as precursor |
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- 2016-03-29 CN CN201610187598.9A patent/CN105694874B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0159085A1 (en) * | 1984-04-12 | 1985-10-23 | Koninklijke Philips Electronics N.V. | Cathode-ray tube |
| CN85102041A (en) * | 1985-04-01 | 1986-10-29 | 菲利浦光灯制造公司 | Cathode ray tube |
| CN1643640A (en) * | 2002-03-28 | 2005-07-20 | 株式会社东芝 | X-ray image tube, x-ray image tube device and x-ray device |
| CN1974885A (en) * | 2006-11-16 | 2007-06-06 | 同济大学 | Low temperature process of preparing RE borate crystal with oxide as precursor |
Non-Patent Citations (3)
| Title |
|---|
| RADHA VELCHURI等: "Low temperature preparation and characterization of In1-xLnxBO3 (x = 0.0 and 0.05； Ln = Gd, Eu, Dy and Sm):ESR of In0.95Gd0.05BO3 and emission of In0.95Eu0.05BO3", 《SPECTROCHIMICA ACTA PART A》 * |
| YUHUA WANG等: "Synthesis and photoluminescence of Eu3+-doped (Y,Gd)BO3 phosphors by a mild hydrothermal process", 《JOURNAL OF CRYSTAL GROWTH》 * |
| 郑灵芝等: "InBO3：Eu3+荧光粉的制备及光谱特性", 《贵州化工》 * |
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