CN104745182A - Neodymium-doped chlorogermanate up-conversion phosphor and preparation method thereof - Google Patents

Neodymium-doped chlorogermanate up-conversion phosphor and preparation method thereof Download PDF

Info

Publication number
CN104745182A
CN104745182A CN201310733165.5A CN201310733165A CN104745182A CN 104745182 A CN104745182 A CN 104745182A CN 201310733165 A CN201310733165 A CN 201310733165A CN 104745182 A CN104745182 A CN 104745182A
Authority
CN
China
Prior art keywords
gecl
conversion phosphor
xnd
germanic acid
calcination
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201310733165.5A
Other languages
Chinese (zh)
Inventor
周明杰
陈吉星
王平
张振华
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
Original Assignee
Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Oceans King Lighting Science and Technology Co Ltd, Shenzhen Oceans King Lighting Engineering Co Ltd filed Critical Oceans King Lighting Science and Technology Co Ltd
Priority to CN201310733165.5A priority Critical patent/CN104745182A/en
Publication of CN104745182A publication Critical patent/CN104745182A/en
Pending legal-status Critical Current

Links

Landscapes

  • Luminescent Compositions (AREA)

Abstract

The invention discloses a neodymium-doped chlorogermanate up-conversion phosphor and a preparation method thereof. The up-conversion phosphor has a general chemical formula of R2GeCl6: xNd<3+>, wherein R is Li, Na, K, Rb or Cs and x is in a range of 0.01 to 0.08. The neodymium-doped chlorogermanate R2GeCl6: xNd<3+> up-conversion phosphor prepared in the invention can realize emission of blue short wave light under excitation of infrared-to-green long wave radiation.

Description

Neodymium doping chlorine germanic acid up-conversion phosphor and preparation method thereof
Technical field
The present invention relates to a kind of fluorescent material field, particularly relate to a kind of neodymium doping chlorine germanic acid up-conversion phosphor and preparation method thereof.
Background technology
The full name Organic Light Emitting Diode of OLED, Organic Light Emitting Diode.It has a lot of advantages, and its unit construction is simple, and production cost is cheap, and self luminous characteristic, adds that the reaction times of OLED is short, more have flexible characteristic, makes its range of application extremely wide.But because the OLED blue light material obtaining stability and high efficiency is at present more difficult, significantly limit the development of white light OLED device and light source industry.
Upconverting fluorescent material can launch visible ray under long wave (as infrared) radiation excitation, even UV-light, is with a wide range of applications in the field such as optical fiber communication technology, fibre amplifier, 3 D stereo display, biomolecules fluorescence labelling, infrared detective.But be prepared into the field that fluorescent material is applied to OLED, still rarely seen report.
Summary of the invention
Based on the problems referred to above, invent problem to be solved and be to provide a kind of chemical general formula to be R 2geCl 6: xNd 3+neodymium doping chlorine germanic acid up-conversion phosphor.
Technical scheme of the present invention is as follows:
Neodymium doping chlorine germanic acid up-conversion phosphor provided by the invention, its chemical general formula is R 2geCl 6: xNd 3+, this up-conversion phosphor adopts following steps to obtain:
(1) be, R by chemical general formula 2geCl 6: xNd 3+in chemical element metering ratio, take RCl, GeCl 4and NdCl 3powder, grinds 20 ~ 60 minutes, obtains uniform powder presoma in corundum mortar;
(2), by the presoma of step (1) put into retort furnace with 800 ~ 1100 DEG C of calcinations 0.5 ~ 5 hour, be then cooled to 100 ~ 300 DEG C, be incubated after 0.5 ~ 3 hour, furnace cooling, to room temperature, obtains block materials;
(3), block materials pulverize, obtaining chemical general formula is R 2geCl 6: xNd 3+described neodymium doping chlorine germanic acid up-conversion phosphor;
Wherein, R 2geCl 6: xNd 3+in, R is Li, Na, K, Rb or Cs; X value is 0.01 ~ 0.08.
Preferred embodiment, in step (1), material powder milling time in corundum mortar is 40 minutes.
Preferred embodiment, in step (2), presoma puts into retort furnace, and calcination temperature is 950 DEG C, and calcination time is 3 hours; After calcination, cooling temperature is 200 DEG C, and cooling soaking time is 2 hours.
Preferred embodiment, in step (3), R 2geCl 6: xNd 3+in x value be 0.05.
The preparation method that the present invention also provides above-mentioned neodymium to adulterate chlorine germanic acid up-conversion phosphor, comprises the steps to obtain:
(1) be, R by chemical general formula 2geCl 6: xNd 3+in chemical element metering ratio, take RCl, GeCl 4and NdCl 3powder, grinds 20 ~ 60 minutes, obtains uniform powder presoma in corundum mortar;
(2), by the presoma of step (1) put into retort furnace with 800 ~ 1100 DEG C of calcinations 0.5 ~ 5 hour, be then cooled to 100 ~ 300 DEG C, be incubated after 0.5 ~ 3 hour, furnace cooling, to room temperature, obtains block materials;
(3), block materials pulverize, obtaining chemical general formula is R 2geCl 6: xNd 3+described neodymium doping chlorine germanic acid up-conversion phosphor;
Wherein, R 2geCl 6: xNd 3+in, R is Li, Na, K, Rb or Cs; X value is 0.01 ~ 0.08.
Neodymium doping chlorine germanic acid R prepared by the present invention 2geCl 6: xNd 3+up-conversion phosphor, can realize inspiring blue light shortwave by the infrared long-wave radiation to green glow luminous; Nd is important rare earth element, and the energy level transition of its 4f electronics in f-f configuration or between f-d all can give off visible ray; In body series, Nd 3+the energy that ionic absorption matrix passes over, energy level 2p 3/2→ 4i 15/2transition radiation go out the glow peak of 469 blue lights.Therefore, this fluorescent material can make up the deficiency of blue light material in display at present and luminescent material.
In addition, the method for preparation is simple, is with low costly applicable to production, and reaction process, without three industrial wastes, belongs to environmental protection, less energy-consumption, high benefit industry.
Accompanying drawing explanation
Fig. 1 is the photoluminescence spectra graphic representation of the neodymium doping chlorine germanic acid up-conversion phosphor that embodiment 1 obtains.Embodiment
Below in conjunction with accompanying drawing, preferred embodiment of the present invention is described in further detail.
Embodiment 1: select LiCl, GeCl 4and NdCl 3powder, its mol ratio is 2mmol, 1mmol, 0.05mmol, in corundum mortar, grinding makes its Homogeneous phase mixing in 40 minutes, then calcination 3 hours at 950 DEG C, is then cooled to 200 DEG C to be incubated 2 hours, furnace cooling takes out to room temperature again, and obtain block materials, can obtain chemical general formula after pulverizing is Li 2geCl 6: 0.05Nd 3+up-conversion phosphor.
Fig. 1 is the photoluminescence spectra graphic representation of the neodymium doping chlorine germanic acid up-conversion phosphor that embodiment 1 obtains; Excitation wavelength is 796nm.That the glow peak of the 469nm obtained is corresponding is Nd 3+ion 2p 3/2→ 4i 15/2transition radiation luminous.
Embodiment 2: select LiCl, GeCl 4and NdCl 3powder, its mol ratio is 2mmol, 1mmol, 0.01mmol, in corundum mortar, grinding makes its Homogeneous phase mixing in 20 minutes, then calcination 0.5 hour at 1100 DEG C, then 100 DEG C are cooled to be incubated 3 hours, furnace cooling takes out to room temperature again, and obtain block materials, can obtain chemical general formula after pulverizing is Li 2geCl 6: 0.01Nd 3+up-conversion phosphor.
Embodiment 3: select LiCl, GeCl 4and NdCl 3powder, its mol ratio is 2mmol, 1mmol, 0.08mmol, in corundum mortar, grinding makes its Homogeneous phase mixing in 60 minutes, then calcination 5 hours at 800 DEG C, is then cooled to 300 DEG C to be incubated 0.5 hour, furnace cooling takes out to room temperature again, and obtain block materials, can obtain chemical general formula after pulverizing is Li 2geCl 6: 0.08Nd 3+up-conversion phosphor.
Embodiment 4: select NaCl, GeCl 4and NdCl 3powder, its mol ratio is 2mmol, 1mmol, 0.05mmol, in corundum mortar, grinding makes its Homogeneous phase mixing in 40 minutes, then calcination 3 hours at 950 DEG C, is then cooled to 200 DEG C to be incubated 2 hours, furnace cooling takes out to room temperature again, and obtain block materials, can obtain chemical general formula after pulverizing is Na 2geCl 6: 0.05Nd 3+up-conversion phosphor.
Embodiment 5: select NaCl, GeCl 4and NdCl 3powder, its mol ratio is 2mmol, 1mmol, 0.01mmol, in corundum mortar, grinding makes its Homogeneous phase mixing in 20 minutes, then calcination 0.5 hour at 1100 DEG C, then 100 DEG C are cooled to be incubated 3 hours, furnace cooling takes out to room temperature again, and obtain block materials, can obtain chemical general formula after pulverizing is Na 2geCl 6: 0.01Nd 3+up-conversion phosphor.
Embodiment 6: select NaCl, GeCl 4and NdCl 3powder, its mol ratio is 2mmol, 1mmol, 0.08mmol, in corundum mortar, grinding makes its Homogeneous phase mixing in 60 minutes, then calcination 5 hours at 800 DEG C, is then cooled to 300 DEG C to be incubated 0.5 hour, furnace cooling takes out to room temperature again, and obtain block materials, can obtain chemical general formula after pulverizing is Na 2geCl 6: 0.08Nd 3+up-conversion phosphor.
Embodiment 7: select KCl, GeCl 4and NdCl 3powder, its mol ratio is 2mmol, 1mmol, 0.05mmol, in corundum mortar, grinding makes its Homogeneous phase mixing in 40 minutes, then calcination 3 hours at 950 DEG C, is then cooled to 200 DEG C to be incubated 2 hours, furnace cooling takes out to room temperature again, and obtain block materials, can obtain chemical general formula after pulverizing is K 2geCl 6: 0.05Nd 3+up-conversion phosphor.
Embodiment 8: select KCl, GeCl 4and NdCl 3powder, its mol ratio is 2mmol, 1mmol, 0.01mmol, in corundum mortar, grinding makes its Homogeneous phase mixing in 20 minutes, then calcination 0.5 hour at 1100 DEG C, is then cooled to 100 DEG C to be incubated 3 hours, furnace cooling takes out to room temperature again, and obtain block materials, can obtain chemical general formula after pulverizing is K 2geCl 6: 0.01Nd 3+up-conversion phosphor.
Embodiment 9: select KCl, GeCl 4and NdCl 3powder, its mol ratio is 2mmol, 1mmol, 0.08mmol, in corundum mortar, grinding makes its Homogeneous phase mixing in 60 minutes, then calcination 5 hours at 800 DEG C, is then cooled to 300 DEG C to be incubated 0.5 hour, furnace cooling takes out to room temperature again, and obtain block materials, can obtain chemical general formula after pulverizing is K 2geCl 6: 0.08Nd 3+up-conversion phosphor.
Embodiment 10: select RbCl, GeCl 4and NdCl 3powder, its mol ratio is 2mmol, 1mmol, 0.05mmol, in corundum mortar, grinding makes its Homogeneous phase mixing in 40 minutes, then calcination 3 hours at 950 DEG C, is then cooled to 200 DEG C to be incubated 2 hours, furnace cooling takes out to room temperature again, and obtain block materials, can obtain chemical general formula after pulverizing is Rb 2geCl 6: 0.05Nd 3+up-conversion phosphor.
Embodiment 11: select RbCl, GeCl 4and NdCl 3powder, its mol ratio is 2mmol, 1mmol, 0.01mmol, in corundum mortar, grinding makes its Homogeneous phase mixing in 20 minutes, then calcination 0.5 hour at 1100 DEG C, then 100 DEG C are cooled to be incubated 3 hours, furnace cooling takes out to room temperature again, and obtain block materials, can obtain chemical general formula after pulverizing is Rb 2geCl 6: 0.01Nd 3+up-conversion phosphor.
Embodiment 12: select RbCl, GeCl 4and NdCl 3powder, its mol ratio is 2mmol, 1mmol, 0.08mmol, in corundum mortar, grinding makes its Homogeneous phase mixing in 60 minutes, then calcination 5 hours at 800 DEG C, is then cooled to 300 DEG C to be incubated 0.5 hour, furnace cooling takes out to room temperature again, and obtain block materials, can obtain chemical general formula after pulverizing is Rb 2geCl 6: 0.08Nd 3+up-conversion phosphor.
Embodiment 13: select CsCl, GeCl 4and NdCl 3powder, its mol ratio is 2mmol, 1mmol, 0.05mmol, in corundum mortar, grinding makes its Homogeneous phase mixing in 40 minutes, then calcination 3 hours at 950 DEG C, is then cooled to 200 DEG C to be incubated 2 hours, furnace cooling takes out to room temperature again, and obtain block materials, can obtain chemical general formula after pulverizing is Cs 2geCl 6: 0.05Nd 3+up-conversion phosphor.
Embodiment 14: select CsCl, GeCl 4and NdCl 3powder, its mol ratio is 2mmol, 1mmol, 0.01mmol, in corundum mortar, grinding makes its Homogeneous phase mixing in 20 minutes, then calcination 0.5 hour at 1100 DEG C, then 100 DEG C are cooled to be incubated 3 hours, furnace cooling takes out to room temperature again, and obtain block materials, can obtain chemical general formula after pulverizing is Cs 2geCl 6: 0.01Nd 3+up-conversion phosphor.
Embodiment 15: select CsCl, GeCl 4and NdCl 3powder, its mol ratio is 2mmol, 1mmol, 0.08mmol, in corundum mortar, grinding makes its Homogeneous phase mixing in 60 minutes, then calcination 5 hours at 800 DEG C, is then cooled to 300 DEG C to be incubated 0.5 hour, furnace cooling takes out to room temperature again, and obtain block materials, can obtain chemical general formula after pulverizing is Cs 2geCl 6: 0.08Nd 3+up-conversion phosphor.
Should be understood that, the above-mentioned statement for present pre-ferred embodiments is comparatively detailed, and therefore can not think the restriction to scope of patent protection of the present invention, scope of patent protection of the present invention should be as the criterion with claims.

Claims (8)

1. a neodymium doping chlorine germanic acid up-conversion phosphor, it is characterized in that, its chemical general formula is R 2geCl 6: xNd 3+, this up-conversion phosphor adopts following steps to obtain:
(1) be, R by chemical general formula 2geCl 6: xNd 3+in chemical element metering ratio, take RCl, GeCl 4and NdCl 3powder, grinds 20 ~ 60 minutes, obtains uniform powder presoma in corundum mortar;
(2), by the presoma of step (1) put into retort furnace with 800 ~ 1100 DEG C of calcinations 0.5 ~ 5 hour, be then cooled to 100 ~ 300 DEG C, be incubated after 0.5 ~ 3 hour, furnace cooling, to room temperature, obtains block materials;
(3), block materials pulverize, obtaining chemical general formula is R 2geCl 6: xNd 3+described neodymium doping chlorine germanic acid up-conversion phosphor;
Wherein, R 2geCl 6: xNd 3+in, R is Li, Na, K, Rb or Cs; X value is 0.01 ~ 0.08.
2. neodymium doping chlorine germanic acid up-conversion phosphor according to claim 1, it is characterized in that, in step (1), material powder milling time in corundum mortar is 40 minutes.
3. neodymium doping chlorine germanic acid up-conversion phosphor according to claim 1, it is characterized in that, in step (2), presoma puts into retort furnace, and calcination temperature is 950 DEG C, and calcination time is 3 hours; After calcination, cooling temperature is 200 DEG C, and cooling soaking time is 2 hours.
4. neodymium doping chlorine germanic acid up-conversion phosphor according to claim 1, is characterized in that, in step (3), and R 2geCl 6: xNd 3+in x value be 0.05.
5. a preparation method for neodymium doping chlorine germanic acid up-conversion phosphor, is characterized in that, comprise the steps to obtain:
(1) be, R by chemical general formula 2geCl 6: xNd 3+in chemical element metering ratio, take RCl, GeCl 4and NdCl 3powder, grinds 20 ~ 60 minutes, obtains uniform powder presoma in corundum mortar;
(2), by the presoma of step (1) put into retort furnace with 800 ~ 1100 DEG C of calcinations 0.5 ~ 5 hour, be then cooled to 100 ~ 300 DEG C, be incubated after 0.5 ~ 3 hour, furnace cooling, to room temperature, obtains block materials;
(3), block materials pulverize, obtaining chemical general formula is R 2geCl 6: xNd 3+described neodymium doping chlorine germanic acid up-conversion phosphor;
Wherein, R 2geCl 6: xNd 3+in, R is Li, Na, K, Rb or Cs; X value is 0.01 ~ 0.08.
6. the preparation method of neodymium doping chlorine germanic acid up-conversion phosphor according to claim 5, it is characterized in that, in step (1), material powder milling time in corundum mortar is 40 minutes.
7. the preparation method of neodymium doping chlorine germanic acid up-conversion phosphor according to claim 5, it is characterized in that, in step (2), presoma puts into retort furnace, and calcination temperature is 950 DEG C, and calcination time is 3 hours; After calcination, cooling temperature is 200 DEG C, and cooling soaking time is 2 hours.
8. the preparation method of neodymium doping chlorine germanic acid up-conversion phosphor according to claim 5, is characterized in that, in step (3), and R 2geCl 6: xNd 3+in x value be 0.05.
CN201310733165.5A 2013-12-26 2013-12-26 Neodymium-doped chlorogermanate up-conversion phosphor and preparation method thereof Pending CN104745182A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201310733165.5A CN104745182A (en) 2013-12-26 2013-12-26 Neodymium-doped chlorogermanate up-conversion phosphor and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201310733165.5A CN104745182A (en) 2013-12-26 2013-12-26 Neodymium-doped chlorogermanate up-conversion phosphor and preparation method thereof

Publications (1)

Publication Number Publication Date
CN104745182A true CN104745182A (en) 2015-07-01

Family

ID=53585453

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201310733165.5A Pending CN104745182A (en) 2013-12-26 2013-12-26 Neodymium-doped chlorogermanate up-conversion phosphor and preparation method thereof

Country Status (1)

Country Link
CN (1) CN104745182A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106118647A (en) * 2016-06-13 2016-11-16 郑甘裕 A kind of neodymium doping chlorine germanate up-conversion luminescent material, preparation method and applications

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106118647A (en) * 2016-06-13 2016-11-16 郑甘裕 A kind of neodymium doping chlorine germanate up-conversion luminescent material, preparation method and applications

Similar Documents

Publication Publication Date Title
CN103045245B (en) Praseodymium ytterbium codope titanium dioxide up-conversion luminescent material, preparation method and application thereof
CN102952543B (en) Thulium-holmium co-doped zirconia upconversion phosphor and preparation method thereof
CN103421491B (en) Terbium ytterbium codoped C 12 A 7 base up-conversion luminescent material, preparation method and Organic Light Emitting Diode
CN103059858B (en) Yttrium silicate upconversion luminous fluorescent powder, preparation method and application thereof
CN104745182A (en) Neodymium-doped chlorogermanate up-conversion phosphor and preparation method thereof
CN104927852A (en) Upconversion fluorescent powder on zirconium-gallium sulphide basal body and preparation method of upconversion fluorescent powder
CN104650882A (en) Terbium/ytterbium-codoped alkali gallium tungstate up-conversion luminescent material, preparation method and application thereof
CN103450896A (en) Thulium-doped fluoroaluminate up-conversion fluorescent powder and preparation method thereof
CN103059844B (en) Sulfide upconversion luminous fluorescent powder, preparation method and application thereof
CN103045253A (en) Thulium doped lithium lanthanum molybdate up-conversion luminescent material, preparation method and application thereof
CN103965908A (en) Dysprosium doped phosphate tellurite glass upconversion luminescent material, and preparation method and application thereof
CN103045243B (en) Praseodymium and ytterbium codope fluoborate glass up-conversion luminescent material and preparation method and application thereof
CN103059853B (en) Titanate phosphors for up-conversion luminescence, and preparation method and application thereof
CN104342148A (en) Thiotungstate fluorescent powder as well as preparation method and application thereof
CN103059867B (en) Tellurate phosphors for up-conversion luminescence, and preparation method and application thereof
CN103045237B (en) Neodymium-ytterbium double-doped barium chloride up-conversion luminescent material as well as preparation method and application thereof
CN103059866B (en) Neodymium ytterbium doped halide upconversion luminous fluorescent powder, preparation method and application thereof
CN103059851B (en) Bismuthate upconversion luminous fluorescent powder, preparation method and application thereof
CN104650910A (en) Praseodymium-doped cerium phosphate up-conversion luminescent material, and preparation method and application thereof
CN104419418A (en) Zirconium boron oxide up-conversion luminescence phosphor and preparation method and application thereof
CN103059845B (en) Germinate phosphors for up-conversion luminescence, and preparation method and application thereof
CN104342150A (en) Neodymium-ytterbium codoped thiomolybdate up-conversion luminescent material and preparation method thereof, and organic light-emitting diode
CN103045244B (en) Dysprosium doped barium titanium glass up-conversion luminescent material, preparation method and application thereof
CN104650866A (en) Thulium doped germanium sulfide chloro-alkaline salt glass upconversion luminescence material, and preparation method and application thereof
CN103045240A (en) Thulium doped strontium aluminate up-conversion luminescent material, preparation method and application thereof

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
WD01 Invention patent application deemed withdrawn after publication
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20150701