CN104745183A - Holmium-doped chlorogermanate up-conversion phosphor and preparation method thereof - Google Patents

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

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CN104745183A
CN104745183A CN201310733223.4A CN201310733223A CN104745183A CN 104745183 A CN104745183 A CN 104745183A CN 201310733223 A CN201310733223 A CN 201310733223A CN 104745183 A CN104745183 A CN 104745183A
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conversion phosphor
gecl
xho
germanate
ammoniacal liquor
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周明杰
陈吉星
王平
张振华
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Abstract

The invention discloses a holmium-doped chlorogermanate up-conversion phosphor and apreparation method thereof. The up-conversion phosphor has a general chemical formula of R2GeCl6: xHo<3+>, wherein x is in a range of 0.01 to 0.08. The holmium-doped chlorogermanate up-conversion phosphor prepared in the invention can realize light emission under the excitation of infrared-to-green long-wave radiation, and an obtained luminescent peak at 490 nm correspondes to transition radiation luminescence of Ho<3+> ions from <5>F3 to <5>I8.

Description

Up-conversion phosphor of holmium doping chlorine germanate and preparation method thereof
Technical field
The present invention relates to a kind of fluorescent material field, particularly relate to up-conversion phosphor of a kind of holmium doping chlorine germanate 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: xHo 3+the up-conversion phosphor of holmium doping chlorine germanate.
Technical scheme of the present invention is as follows:
The up-conversion phosphor of holmium doping chlorine germanate provided by the invention, its chemical general formula is R 2geCl 6: xHo 3+, this up-conversion phosphor adopts following steps to obtain:
(1) be, R by chemical general formula 2geCl 6: xHo 3+in chemical element metering ratio, take R 2o, GeO and Ho 2o 3in the hydrochloric acid that powder is dissolved in 0.01 ~ 0.5mol/L or perchloric acid, form mixing solutions;
(2), in the mixing solutions of step (1) drip oxalic acid and ammoniacal liquor simultaneously, and constantly stir, until throw out no longer produces, continue to drip ammoniacal liquor, about the PH to 8 in regulator solution, leave standstill 1 ~ 5 hour, make precipitation complete; Wherein, oxalic acid is as precipitation agent; Ammoniacal liquor plays the pH value effect in balanced reaction liquid, does not introduce other positively charged ions;
(3) throw out, in filtration step (2), and obtain sample with after ethanol and distilled water repetitive scrubbing;
(4), step (3) is washed after the sample that obtains be placed in 900 ~ 1400 DEG C at roasting after 0.5 ~ 3 hour, obtaining chemical general formula is R 2geCl 6: xHo 3+the up-conversion phosphor of described holmium doping chlorine germanate; Wherein, R 2geCl 6: xHo 3+in x value be 0.01 ~ 0.08.
As preferred embodiment, in step (2), time of repose is 2 hours.
As preferred embodiment, in step (4), be 1200 DEG C to the maturing temperature of sample, roasting time is 2 hours.
As preferred embodiment, in step (4), R 2geCl 6: xHo 3+in x value be 0.05.
The preparation method of the up-conversion phosphor that the present invention also provides above-mentioned holmium to adulterate chlorine germanate, comprises the steps to obtain:
(1) be, R by chemical general formula 2geCl 6: xHo 3+in chemical element metering ratio, take R 2o, GeO and Ho 2o 3in the hydrochloric acid that powder is dissolved in 0.01 ~ 0.5mol/L or perchloric acid, form mixing solutions;
(2), in the mixing solutions of step (1) drip oxalic acid and ammoniacal liquor simultaneously, and constantly stir, until throw out no longer produces, continue to drip ammoniacal liquor, about the PH to 8 in regulator solution, leave standstill 1 ~ 5 hour, make precipitation complete;
(3) throw out, in filtration step (2), and obtain sample with after ethanol and distilled water repetitive scrubbing;
(4), step (3) is washed after the sample that obtains be placed in 900 ~ 1400 DEG C at roasting 0.5 ~ 3 hour, obtaining chemical general formula is R 2geCl 6: xHo 3+the up-conversion phosphor of described holmium doping chlorine germanate; Wherein, R 2geCl 6: xHo 3+in x value be 0.01 ~ 0.08.
The present invention's coprecipitation method has prepared holmium doping chlorine germanate R 2geCl 6: xHo 3+up-conversion phosphor, can realize being excited by the infrared long-wave radiation to green glow, and that the glow peak of the 490nm obtained is corresponding is Ho 3+ion 5f 3→ 5i 8transition radiation luminous, its relative luminous intensity is about 240.Chemical coprecipitation used is prepared fluorescent material and is had the advantages such as composition is even, purity is high, particle is thin, synthesis temperature is low.
Accompanying drawing explanation
Fig. 1 is the photoluminescence spectra graphic representation of the up-conversion phosphor of the holmium doping chlorine germanate that embodiment 1 obtains.
Embodiment
Below in conjunction with accompanying drawing, preferred embodiment of the present invention is described in further detail.
Embodiment 1: take Li 2o, GeO 2and Ho 2o 3powder, is respectively 0.95mmol, 1mmol, 0.025mmol, after being all dissolved in the hydrochloric acid HCl of 0.5mol/L, instills oxalic acid and ammoniacal liquor while stirring simultaneously.Mixing solutions is regeneration throw out not, continues to drip ammoniacal liquor, and pH value is adjusted to about 8, leaves standstill and within 2 hours, makes precipitation complete, and then throw out dehydrated alcohol and distilled water repetitive scrubbing, finally roasting 2 hours at 1000 DEG C, obtaining chemical general formula is Li 2geCl 6: 0.05Ho 3+up-conversion phosphor.
Fig. 1 is the photoluminescence spectra graphic representation of the up-conversion phosphor of the holmium doping chlorine germanate that embodiment 1 obtains; Excitation wavelength is 796nm.That the glow peak of the 475nm obtained is corresponding is Ho 3+ion 1g 4→ 3h 6transition radiation luminous, its relative luminous intensity is about 240.
Embodiment 2: take Li 2o, GeO 2and Ho 2o 3powder, is respectively 0.82mmol, after 1mmol, 0.04mmol are all dissolved in the hydrochloric acid HCl of 0.03mol/L, instills oxalic acid and ammoniacal liquor while stirring simultaneously.Mixing solutions is regeneration throw out not, continues to drip ammoniacal liquor, and pH value is adjusted to about 8, leaves standstill and within 1 hour, makes precipitation complete, and then throw out dehydrated alcohol and distilled water repetitive scrubbing, finally roasting 3 hours at 900 DEG C, obtaining chemical general formula is Li 2geCl 6: 0.08Ho 3+up-conversion phosphor.
Embodiment 3: take Li 2o, GeO 2powder, is respectively 0.99mmol, 1mmol, 0.005mmol, after being all dissolved in the hydrochloric acid HCl of 0.01mol/L, instills oxalic acid and ammoniacal liquor while stirring simultaneously.Mixing solutions is regeneration throw out not, continues to drip ammoniacal liquor, and pH value is adjusted to about 8, leaves standstill and within 5 hours, makes precipitation complete, and then throw out dehydrated alcohol and distilled water repetitive scrubbing, finally roasting 0.5 hour at 1300 DEG C, obtaining chemical general formula is Li 2geCl 6: 0.01Ho 3+up-conversion phosphor.
Embodiment 4: take Na 2o, GeO 2and Ho 2o 3powder, is respectively 0.95mmol, 1mmol, 0.025mmol, after being all dissolved in the hydrochloric acid HCl of 0.5mol/L, instills oxalic acid and ammoniacal liquor while stirring simultaneously.Mixing solutions is regeneration throw out not, continues to drip ammoniacal liquor, and pH value is adjusted to about 8, leaves standstill and within 2 hours, makes precipitation complete, and then throw out dehydrated alcohol and distilled water repetitive scrubbing, finally roasting 2 hours at 1000 DEG C, obtaining chemical general formula is Na 2geCl 6: 0.05Ho 3+up-conversion phosphor.
Embodiment 5: take Na 2o, GeO 2and Yb 2o 3powder, is respectively 0.82mmol, after 1mmol, 0.04mmol are all dissolved in the hydrochloric acid HCl of 0.3mol/L, instills oxalic acid and ammoniacal liquor while stirring simultaneously.Mixing solutions is regeneration throw out not, continues to drip ammoniacal liquor, and pH value is adjusted to about 8, leaves standstill and within 1 hour, makes precipitation complete, and then throw out dehydrated alcohol and distilled water repetitive scrubbing, finally roasting 3 hours at 900 DEG C, obtaining chemical general formula is Na 2geCl 6: 0.08Ho 3+up-conversion phosphor.
Embodiment 6: take Na 2o, GeO 2powder, is respectively 0.99mmol, 1mmol, 0.005mmol, after being all dissolved in the hydrochloric acid HCl of 0.01mol/L, instills oxalic acid and ammoniacal liquor while stirring simultaneously.Mixing solutions is regeneration throw out not, continues to drip ammoniacal liquor, and pH value is adjusted to about 8, leaves standstill and within 5 hours, makes precipitation complete, and then throw out dehydrated alcohol and distilled water repetitive scrubbing, finally roasting 0.5 hour at 1300 DEG C, obtaining chemical general formula is Na 2geCl 6: 0.01Ho 3+up-conversion phosphor.
Embodiment 7: take K 2o, GeO 2and Ho 2o 3powder, is respectively 0.95mmol, 1mmol, 0.025mmol, is all dissolved in the perchloric acid HClO of 0.5mol/L 4after, instill oxalic acid and ammoniacal liquor while stirring simultaneously.Mixing solutions is regeneration throw out not, continues to drip ammoniacal liquor, and pH value is adjusted to about 8, leaves standstill and within 2 hours, makes precipitation complete, and then throw out dehydrated alcohol and distilled water repetitive scrubbing, finally roasting 2 hours at 1000 DEG C, obtaining chemical general formula is K 2geCl 6: 0.05Ho 3+up-conversion phosphor.
Embodiment 8: take K 2o, GeO 2and Ho 2o 3powder, is respectively 0.82mmol, after 1mmol, 0.04mmol are all dissolved in the hydrochloric acid HCl of 0.01mol/L, instills oxalic acid and ammoniacal liquor while stirring simultaneously.Mixing solutions is regeneration throw out not, continues to drip ammoniacal liquor, and pH value is adjusted to about 8, leaves standstill and within 1 hour, makes precipitation complete, and then throw out dehydrated alcohol and distilled water repetitive scrubbing, finally roasting 3 hours at 900 DEG C, obtaining chemical general formula is K 2geCl 6: 0.08Ho 3+up-conversion phosphor.
Embodiment 9: take K 2o, GeO 2powder, is respectively 0.99mmol, 1mmol, 0.005mmol, after being all dissolved in the hydrochloric acid HCl of 0.5mol/L, instills oxalic acid and ammoniacal liquor while stirring simultaneously.Mixing solutions is regeneration throw out not, continues to drip ammoniacal liquor, and pH value is adjusted to about 8, leaves standstill and within 5 hours, makes precipitation complete, and then throw out dehydrated alcohol and distilled water repetitive scrubbing, finally roasting 0.5 hour at 1300 DEG C, obtaining chemical general formula is K 2geCl 6: 0.01Ho 3+up-conversion phosphor.
Embodiment 10: take Rb 2o, GeO 2and Ho 2o 3powder, is respectively 0.95mmol, 1mmol, 0.025mmol, is all dissolved in the perchloric acid HClO of 0.01mol/L 4after, instill oxalic acid and ammoniacal liquor while stirring simultaneously.Mixing solutions is regeneration throw out not, continues to drip ammoniacal liquor, and pH value is adjusted to about 8, leaves standstill and within 2 hours, makes precipitation complete, and then throw out dehydrated alcohol and distilled water repetitive scrubbing, finally roasting 2 hours at 1000 DEG C, obtaining chemical general formula is Rb 2geCl 6: 0.05Ho 3+up-conversion phosphor.
Embodiment 11: take Rb 2o, GeO 2and Ho 2o 3powder, is respectively 0.82mmol, after 1mmol, 0.04mmol are all dissolved in the hydrochloric acid HCl of 0.3mol/L, instills oxalic acid and ammoniacal liquor while stirring simultaneously.Mixing solutions is regeneration throw out not, continues to drip ammoniacal liquor, and pH value is adjusted to about 8, leaves standstill and within 1 hour, makes precipitation complete, and then throw out dehydrated alcohol and distilled water repetitive scrubbing, finally roasting 3 hours at 900 DEG C, obtaining chemical general formula is Rb 2geCl 6: 0.08Ho 3+up-conversion phosphor.
Embodiment 12: take Rb 2o, GeO 2powder, is respectively 0.99mmol, 1mmol, 0.005mmol, after being all dissolved in the hydrochloric acid HCl of 0.01mol/L, instills oxalic acid and ammoniacal liquor while stirring simultaneously.Mixing solutions is regeneration throw out not, continues to drip ammoniacal liquor, and pH value is adjusted to about 8, leaves standstill and within 5 hours, makes precipitation complete, and then throw out dehydrated alcohol and distilled water repetitive scrubbing, finally roasting 0.5 hour at 1300 DEG C, obtaining chemical general formula is Rb 2geCl 6: 0.01Ho 3+up-conversion phosphor.
Embodiment 13: take Cs 2o, GeO 2and Ho 2o 3powder, is respectively 0.95mmol, 1mmol, 0.025mmol, after being all dissolved in the hydrochloric acid HCl of 0.3mol/L, instills oxalic acid and ammoniacal liquor while stirring simultaneously.Mixing solutions is regeneration throw out not, continues to drip ammoniacal liquor, and pH value is adjusted to about 8, leaves standstill and within 2 hours, makes precipitation complete, and then throw out dehydrated alcohol and distilled water repetitive scrubbing, finally roasting 2 hours at 1000 DEG C, obtaining chemical general formula is Cs 2geCl 6: 0.05Ho 3+up-conversion phosphor.
Embodiment 14: take Cs 2o, GeO 2and Ho 2o 3powder, is respectively 0.82mmol, and 1mmol, 0.04mmol are all dissolved in the perchloric acid HClO of 0.3mol/L 4after, instill oxalic acid and ammoniacal liquor while stirring simultaneously.Mixing solutions is regeneration throw out not, continues to drip ammoniacal liquor, and pH value is adjusted to about 8, leaves standstill and within 1 hour, makes precipitation complete, and then throw out dehydrated alcohol and distilled water repetitive scrubbing, finally roasting 3 hours at 900 DEG C, obtaining chemical general formula is Cs 2geCl 6: 0.08Ho 3+up-conversion phosphor.
Embodiment 15: take Cs 2o, GeO 2powder, is respectively 0.99mmol, 1mmol, 0.005mmol, after being all dissolved in the hydrochloric acid HCl of 0.5mol/L, instills oxalic acid and ammoniacal liquor while stirring simultaneously.Mixing solutions is regeneration throw out not, continues to drip ammoniacal liquor, and pH value is adjusted to about 8, leaves standstill and within 5 hours, makes precipitation complete, and then throw out dehydrated alcohol and distilled water repetitive scrubbing, finally roasting 0.5 hour at 1300 DEG C, obtaining chemical general formula is Cs 2geCl 6: 0.01Ho 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 (7)

1. a up-conversion phosphor for holmium doping chlorine germanate, it is characterized in that, its chemical general formula is R 2geCl 6: xHo 3+, this up-conversion phosphor adopts following steps to obtain:
(1) be, R by chemical general formula 2geCl 6: xHo 3+in chemical element metering ratio, take R 2o, GeO and Ho 2o 3in the hydrochloric acid that powder is dissolved in 0.01 ~ 0.5mol/L or perchloric acid, form mixing solutions;
(2), in the mixing solutions of step (1) drip oxalic acid and ammoniacal liquor simultaneously, and constantly stir, until throw out no longer produces, continue to drip ammoniacal liquor, about the PH to 8 in regulator solution, leave standstill 1 ~ 5 hour, make precipitation complete;
(3) throw out, in filtration step (2), and obtain sample with after ethanol and distilled water repetitive scrubbing;
(4), step (3) is washed after the sample that obtains be placed in 900 ~ 1400 DEG C at roasting after 0.5 ~ 3 hour, obtaining chemical general formula is R 2geCl 6: xHo 3+the up-conversion phosphor of described holmium doping chlorine germanate; Wherein, R 2geCl 6: xHo 3+in x value be 0.01 ~ 0.08.
2. the up-conversion phosphor of holmium doping chlorine germanate according to claim 1, it is characterized in that, in step (2), described time of repose is 2 hours.
3. the up-conversion phosphor of holmium doping chlorine germanate according to claim 1, it is characterized in that, in step (4), be 1200 DEG C to the maturing temperature of sample, roasting time is 2 hours.
4. the up-conversion phosphor of holmium doping chlorine germanate according to claim 1, is characterized in that, in step (4), and R 2geCl 6: xHo 3+in x value be 0.05.
5. a preparation method for the up-conversion phosphor of holmium doping chlorine germanate, is characterized in that, comprise the steps to obtain:
(1) be, R by chemical general formula 2geCl 6: xHo 3+in chemical element metering ratio, take R 2o, GeO and Ho 2o 3in the hydrochloric acid that powder is dissolved in 0.01 ~ 0.5mol/L or perchloric acid, form mixing solutions;
(2), in the mixing solutions of step (1) drip oxalic acid and ammoniacal liquor simultaneously, and constantly stir, until throw out no longer produces, continue to drip ammoniacal liquor, about the PH to 8 in regulator solution, leave standstill 1 ~ 5 hour, make precipitation complete;
(3) throw out, in filtration step (2), and obtain sample with after ethanol and distilled water repetitive scrubbing;
(4), step (3) is washed after the sample that obtains be placed in 900 ~ 1400 DEG C at roasting 0.5 ~ 3 hour, obtaining chemical general formula is R 2geCl 6: xHo 3+the up-conversion phosphor of described holmium doping chlorine germanate; Wherein, R 2geCl 6: xHo 3+in x value be 0.01 ~ 0.08.
6. the preparation method of the up-conversion phosphor of holmium doping chlorine germanate according to claim 5, it is characterized in that, in step (4), be 1200 DEG C to the maturing temperature of sample, roasting time is 1 ~ 5 hour.
7. the preparation method of the up-conversion phosphor of holmium doping chlorine germanate according to claim 5, is characterized in that, in step (4), and R 2geCl 6: xHo 3+in x value be 0.05.
CN201310733223.4A 2013-12-26 2013-12-26 Holmium-doped chlorogermanate up-conversion phosphor and preparation method thereof Pending CN104745183A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106010519A (en) * 2016-06-13 2016-10-12 郑甘裕 Chlorine germanate up-conversion luminescent material, preparing method and application

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106010519A (en) * 2016-06-13 2016-10-12 郑甘裕 Chlorine germanate up-conversion luminescent material, preparing method and application

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