CN102433115A - Preparation method for blue light excited warm-color long-afterglow luminescent material - Google Patents

Preparation method for blue light excited warm-color long-afterglow luminescent material Download PDF

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Publication number
CN102433115A
CN102433115A CN2011103548584A CN201110354858A CN102433115A CN 102433115 A CN102433115 A CN 102433115A CN 2011103548584 A CN2011103548584 A CN 2011103548584A CN 201110354858 A CN201110354858 A CN 201110354858A CN 102433115 A CN102433115 A CN 102433115A
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long
blue
preparation
red
afterglow
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CN2011103548584A
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孔哲
席俊华
张尔攀
季振国
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Hangzhou Dianzi University
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Hangzhou Dianzi University
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Priority to CN2011103548584A priority Critical patent/CN102433115A/en
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Abstract

The invention relates to a preparation method for a blue light excited warm-color long-afterglow luminescent material. All types of red luminescent materials at present cannot meet practical requirements because either the luminous intensity is low or the afterglow time is too short, or pollution is caused to the environment. According to the preparation method, a blue light excited CaAl12O9:Mn<2+> red luminescent material is wrapped on the surface of CaAl2O4:Eu<2+> and Nd<3+> blue long-afterglow luminescent powder, and the thickness of the wrapping layer is controlled, so that the aim of 'blue-purple-mauve-red' efficient warm-color long-afterglow luminescence is fulfilled. By adoption of the preparation method, the problem of short afterglow time of a warm-color luminescent material which is directly prepared at present is solved; and the preparation method is a new way for preparing the warm-color long-afterglow luminescent material.

Description

A kind of blue-light excited warm colour long after glow luminous material preparation method
Technical field
The present invention relates to luminescent material, relate in particular to long afterglow luminous material, is a kind of preparation method of warm colour long after glow luminous material, can be widely used in all kinds of noctilucence products of preparation.
Background technology
Long after glow luminous material is one type of important light-light-converting material and energy-storage economical material, and it has special advantages in solar energy converting with aspect utilizing.Can get up storage of solar energy its daytime, and evening is slow release again, is a kind of free of contamination cold light source.This type material can be made a series of noctilucence products such as radioactive paint, luminous printing ink, luminescent fibre, luminescent ceramic, is applied to aspects such as upholstery, secure ID, communications and transportation, military equipment.
Long-afterglow material has been gathered the double dominant of energy-saving and environmental protection, has caused people's extensive concern.Up to now, surpassed 12 h the after time of green of being developed and blue long afterflow material, reached actual request for utilization, applies.But the excitation spectrum of red long afterglow luminous material generally is positioned at the UV-light zone, can not effectively be excited by sunshine.Because its inherent defective, red illuminating material is all can't be equal to materials such as green glow, blue lights aspect luminosity or after time, and it also is in conceptual phase in the long after glow luminous material field.Therefore, research and development high brightness, after time long, environment-friendly, chemical property and stable luminescent property red long afterglow luminous material be problem demanding prompt solution.Solve this problem and just can realize the preparation of the long afterglow luminous product of warm colour that colourity is adjustable.
Summary of the invention
Through literature survey widely, all kinds of red illuminating materials of finding present institute primary study be not luminous intensity not high, be exactly after time too short, perhaps environment is had pollution, all can not reach practical requirement.For this reason; Imagine compound steady persistence blue emitting material and red illuminating material; Utilize blue long afterflow luminescent material to be light source activation emitting red light powder, like this no matter whether the twilight sunset of red light-emitting material itself is enough long, as long as the blue long afterflow material can send light; With its compound red illuminating material also can continue luminous, thereby reach red " steady persistence " luminous purpose.
Blue and the red compound warm colour long after glow luminous material that obtains adopts red illuminating material to wrap up the method for blue-light-emitting powder.In this method; As long as red material parcel thickness is enough thick, red blue material ratio is appropriate, and the light that the blue light material that is wrapped sends can be absorbed by the red illuminating material of outside basically; Obtain purer ruddiness thus, otherwise then can obtain from indigo plant to red warm colour light.But because blue light material is wrapped in red material inside, how extraneous irradiates light gets into the blue-light-emitting core through red illuminating material is a difficult problem that needs solution.This can solve through selecting suitable red illuminating material, and promptly red illuminating material can absorb indigo plant effectively and send ruddiness, can let again the short wavelength light transmission it and excite inner blue long afterflow material.
In sum, for the long after glow luminous material field, through blue long afterflow material and red illuminating material can obtain can be from the blueness to the redness standard long-persistence luminous.Based on the great demand of existing market to long after glow luminous material, realize warm colour long-persistence luminous be an exploration that application prospect is arranged very much.The research of this type of warm colour " steady persistence " luminescent material does not appear in the newspapers at present as yet.
Preparing method's of the present invention basic step is following:
(1) with Ca (NO 3) 2: Al (NO 3) 3Mix than 1:12 with amount of substance, add dissolve with ethanol, a certain amount of Mn (NO mixes 3) 2Continued stirs and adds acetone with Mn (NO 3) 2Dissolving, described Mn (NO 3) 2Amount of substance is Ca (NO 3) 20.01~0.1 of amount of substance.
(2) add CaAl 2O 4: Eu 2+, Nd 3+The blue long afterflow luminescent powder, control Ca (NO 3) 2, Al (NO 3) 3And Mn (NO 3) 2Total mass and CaAl 2O 4: Eu 2+, Nd 3+The ratio of quality be 20~10:1, thorough mixing is even, continues to stir and at 80 ℃ of ethanol evaporation and acetone, prepare dried glue at 80 ℃ of dry 20h then.
(3) dried glue is put into vacuum system, vacuumize, make the pressure of Vakuumkammer be lower than 1 * 10 -1Pa.
(4) unlocking electronic rifle, the energy of electron beam are to regulate between 1KeV~10KeV, and beam current density is at 10mAcm -2~100mAcm -2Between regulate.
(5) electron beam is scanned on dried glue,, make the warm colour long after glow luminous material up to sending macroscopic ruddiness.
Beneficial effect of the present invention: the luminescent powder composition that the packaging method that the present invention adopts obtains is even, and after time is longer than the warm colour luminescent material of directly preparation, can reach more than ten hours, and luminescent chromaticity is adjustable and character is more stable.
The present invention adopts the method for red illuminating material parcel blue-light-emitting powder, as long as the light that the blue light material that is wrapped sends can be absorbed by the red illuminating material of outside basically, the interference of basically eliminate blue light obtains purer ruddiness thus.Being equipped with the warm colour luminescent material with the traditional mixing legal system compares and can obtain pure red light more.
Embodiment
Describe the present invention in detail based on specific embodiment below, it is more obvious that the object of the invention and effect will become.
Embodiment 1:
(1) with Ca (NO 3) 2: Al (NO 3) 3Mix than 1:12 with amount of substance, add dissolve with ethanol, a certain amount of Mn (NO mixes 3) 2(its amount of substance is Ca (NO 3) 2Amount of substance 0.01) continued stirs and adds acetone it is dissolved.
(2) add CaAl 2O 4: Eu 2+, Nd 3+The blue long afterflow luminescent powder, control (1): the total mass ratio of (2) dry powder is 10:1, and thorough mixing is even, continues to stir and at 80 ℃ of evaporating solvents, prepare dried glue at 80 ℃ of dry 20h then.
(3) dried glue is put into vacuum system, vacuumize, make the pressure of Vakuumkammer be lower than 1 * 10 -1Pa;
(4) unlocking electronic rifle, the energy of electron beam are to regulate between 1KeV~10KeV, and beam current density is at 10mAcm -2~100mAcm -2Between regulate.
(5) electron beam is scanned on dried glue,, make the warm colour long after glow luminous material up to sending macroscopic ruddiness.
Embodiment 2:
(1) with Ca (NO 3) 2: Al (NO 3) 3Mix than 1:12 with amount of substance, add dissolve with ethanol, a certain amount of Mn (NO mixes 3) 2(its amount of substance is Ca (NO 3) 2Amount of substance 0.05) continued stirs and adds acetone it is dissolved.
(2) add CaAl 2O 4: Eu 2+, Nd 3+The blue long afterflow luminescent powder, control (1): the total mass ratio of (2) dry powder is 15:1, and thorough mixing is even, continues to stir and at 80 ℃ of evaporating solvents, prepare dried glue at 80 ℃ of dry 20h then.
(3) dried glue is put into vacuum system, vacuumize, make the pressure of Vakuumkammer be lower than 1 * 10 -1Pa.
(4) unlocking electronic rifle, the energy of electron beam are to regulate between 1KeV~10KeV, and beam current density is at 10mAcm -2~100mAcm -2Between regulate.
(5) electron beam is scanned on dried glue,, make the warm colour long after glow luminous material up to sending macroscopic ruddiness.
Embodiment 3:
(1) with Ca (NO 3) 2: Al (NO 3) 3Mix than 1:12 with amount of substance, add dissolve with ethanol, a certain amount of Mn (NO mixes 3) 2(its amount of substance is Ca (NO 3) 2Amount of substance 0.1) continued stirs and adds acetone it is dissolved.
(2) add CaAl 2O 4: Eu 2+, Nd 3+The blue long afterflow luminescent powder, control (1): the total mass ratio of (2) dry powder is 20:1, and thorough mixing is even, continues to stir and at 80 ℃ of evaporating solvents, prepare dried glue at 80 ℃ of dry 20h then.
(3) dried glue is put into vacuum system, vacuumize, make the pressure of Vakuumkammer be lower than 1 * 10 -1Pa.
(4) unlocking electronic rifle, the energy of electron beam are to regulate between 1KeV~10KeV, and beam current density is at 10mAcm -2~100mAcm -2Between regulate.
(5) electron beam is scanned on dried glue,, make the warm colour long after glow luminous material up to sending macroscopic ruddiness.

Claims (2)

1. blue-light excited warm colour long after glow luminous material preparation method; It is characterized in that: carry out compoundly through blue-light excited red illuminating material and blue long afterflow luminescent material, utilize blue light that red illuminating material long-acting excited and realize that the warm colour that red long-afterglow is luminous and colourity is adjustable is long-persistence luminous.
2. according to the described preparation method of claim 1, it is characterized in that the concrete steps of this method are following:
(1) with Ca (NO 3) 2: Al (NO 3) 3Mix than 1:12 with amount of substance, add dissolve with ethanol, a certain amount of Mn (NO mixes 3) 2Continued stirs and adds acetone with Mn (NO 3) 2Dissolving, described Mn (NO 3) 2Amount of substance is Ca (NO 3) 20.01~0.1 of amount of substance;
(2) add CaAl 2O 4: Eu 2+, Nd 3+The blue long afterflow luminescent powder, control Ca (NO 3) 2, Al (NO 3) 3And Mn (NO 3) 2Total mass and CaAl 2O 4: Eu 2+, Nd 3+The ratio of quality be 20~10:1, thorough mixing is even, continues to stir and at 80 ℃ of ethanol evaporation and acetone, prepare dried glue at 80 ℃ of dry 20h then;
(3) dried glue is put into vacuum system, vacuumize, make the pressure of Vakuumkammer be lower than 1 * 10 -1Pa;
(4) unlocking electronic rifle, the energy of electron beam are to regulate between 1KeV~10KeV, and beam current density is at 10mAcm -2~100mAcm -2Between regulate;
(5) electron beam is scanned on dried glue,, make the warm colour long after glow luminous material up to sending macroscopic ruddiness.
CN2011103548584A 2011-11-10 2011-11-10 Preparation method for blue light excited warm-color long-afterglow luminescent material Pending CN102433115A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102732250A (en) * 2012-06-27 2012-10-17 华南理工大学 Red phosphor and preparation method thereof
CN107746708A (en) * 2017-11-02 2018-03-02 杭州显庆科技有限公司 A kind of red long-afterglow phosphor and preparation method thereof

Non-Patent Citations (5)

* Cited by examiner, † Cited by third party
Title
《Electronic Materials Letters》 20100331 Jung Hyun Park et al. Sol-Gel Synthesis of CaAl12O19:Mn Phosphor and Red Luminescence by Near-Ultraviolet/Blue Excitation 第13-15页 1-2 第6卷, 第1期 *
JUNG HYUN PARK ET AL.: "Sol-Gel Synthesis of CaAl12O19:Mn Phosphor and Red Luminescence by Near-Ultraviolet/Blue Excitation", 《ELECTRONIC MATERIALS LETTERS》 *
T. MURATA ET AL.: "Fluorescence properties of Mn4+ in CaAl12O19 compounds as red-emitting phosphor for white LED", 《JOURNAL OF LUMINESCENCE》 *
VIJAY SINGH: "Luminescence and EPR investigations of Mn activated calcium aluminate prepared via combustion method", 《OPTICAL MATERIALS》 *
徐叙瑢等: "《发光学与发光材料》", 31 October 2004, 化学工业出版社 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102732250A (en) * 2012-06-27 2012-10-17 华南理工大学 Red phosphor and preparation method thereof
CN107746708A (en) * 2017-11-02 2018-03-02 杭州显庆科技有限公司 A kind of red long-afterglow phosphor and preparation method thereof
CN107746708B (en) * 2017-11-02 2018-12-04 宁波朗格照明电器有限公司 A kind of red long-afterglow phosphor and preparation method thereof

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Application publication date: 20120502