CN1528858A - Nano fluorescent powder and preparing method thereof - Google Patents
Nano fluorescent powder and preparing method thereof Download PDFInfo
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- CN1528858A CN1528858A CNA2003101112082A CN200310111208A CN1528858A CN 1528858 A CN1528858 A CN 1528858A CN A2003101112082 A CNA2003101112082 A CN A2003101112082A CN 200310111208 A CN200310111208 A CN 200310111208A CN 1528858 A CN1528858 A CN 1528858A
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Abstract
The invention refers to a kind of nano fluorescence powder and the manufacturing method, the nano fluorescence is compound, the chemical composition is: Zn2-x-ySiO4: xMn, yEr, x is not less than 0.01 and not greater than 0.15, y is not less than 0.0001 and not greater than 0.001. the invention uses Mn2+, Er3+ as activation agent, it can upgrades the brightening efficiency of the product, the heat stability is good, the operating life is long, it caters the demand to fluorescence powder brightening performance by PDP: at the same time, it has some effect to shorten the afterglow time. The particles are small, the product has good dispersibility, the brightening performance is excellent. The invention overcomes long afterglow time problem by adding Mn2+ usage and using Mn2+ and Er3+ to activate.
Description
Technical field
The present invention relates to the luminescent material technical field, particularly fluorescent material that in novel backlight sources such as color plasma display (PDP), compact type energy-saving lamp, no mercury neon light, liquid-crystal display, uses and preparation method thereof.
Technical background
Along with advancing by leaps and bounds of science and technology and improving constantly of people's demand, a kind of novel flat-plate indicating meter-chromatic plasma flat-panel monitor (PDP) development becomes the flat panel display of most promising large-screen high-resolution degree rapidly.PDP has advantages such as large size, in light weight and panelized.The PDP principle of work is that the ultraviolet ray that noble gas discharge produces excites three primary colors fluorescent powder luminous, and therefore in the PDP industry, except driving circuit, most important is exactly luminescent material, i.e. fluorescent material.The wavelength of rare gas element emission is positioned at vacuum ultraviolet (VUV) (VUV) in PDP, be 147nm, therefore require well behaved with this understanding fluorescent material to satisfy the demand of PDP industry, but present most PDP producer still continues to use traditional lamp phosphor, caused the performance imperfection of color PDP, for example: the market sale green emitting phosphor that current PDP producer adopts exists that particle is inhomogeneous, particle is bigger than normal etc. and can not finely satisfy the needs of industrial production system screen technological development; Grow, be unfavorable for the serial problems such as dynamic demonstration of display image particularly luminous time of persistence partially.
Summary of the invention
Technical problem to be solved by this invention is: a kind of nano-phosphor and preparation method thereof is provided, and this nano fluorescent powder particles is tiny evenly, luminous efficiency is high, time of persistence is short, Heat stability is good and life-span are long.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: it is a compound, and its chemical formula consists of:
Zn
2-x-ySiO
4:xMn，yEr
Wherein: 0.01≤x≤0.15,0.0001≤y≤0.001;
Its grain diameter 30-100nm.
The method for preparing above-mentioned nano-phosphor, its step comprises:
(1) presses soluble zinc salt or zinc oxide/tetraethoxy=1.85～1.99: 1, soluble manganese salt/Erbium trioxide=20～3000: 1, soluble zinc salt or zinc oxide/soluble manganese salt=5～40: 1 mole ratio, accurately weighing soluble zinc salt or zinc oxide, tetraethoxy, soluble manganese salt, Erbium trioxide;
(2) soluble zinc salt or zinc oxide, soluble manganese salt, Erbium trioxide are mixed put into container;
(3) add 1: 1 nitric acid in said vesse, heated and stirred is to boiling, and the material in the container is fully dissolved; Per 1 gram soluble zinc salt or zinc oxide, soluble manganese salt, Erbium trioxide solid total mass add 4～10 milliliters of nitric acid of 1: 1.
(4) add distilled water, and add solubility promoter---boric acid, the mixed solution in the container is diluted;
(5) in mixed solution, drip tetraethoxy, put into 60-90 ℃ water-bath device after stirring, make it peptization to transparent, spherical colloidal sol and generate;
(6) the above-mentioned colloidal sol of gained is placed 90～150 ℃ far infrared drying oven, make it to be transformed into xerogel;
(7) xerogel of gained was heat-treated in 400～800 ℃ retort furnace 1～4 hour;
(8) after the presoma cooling with the thermal treatment gained, place 800～1200 ℃ hydrogen and nitrogen gas atmosphere stove, sintering is 1～4 hour under the competent condition of assurance reducing atmosphere, obtains fluorescent material product in early stage; Contain H in the hydrogen and nitrogen gas atmosphere stove
210～25%, N
275～90%;
(9) to above-mentioned fluorescent material product adding in early stage dispersion agent---water, place ultrasonic wave to carry out ultra-sonic dispersion and handle;
(10) with after the filtration of the fluorescent material product behind the ultra-sonic dispersion, the loft drier of putting into 30～90 ℃ is dry, obtains required product.
The present invention adopts Mn
2+, Er
3+As coactivator, can greatly improve the quantum luminous efficiency of fluorescent material product, Heat stability is good, the life-span is long, satisfies color PDP to the light-emitting phosphor performance demands; Simultaneously to also having played certain effect the time of persistence that shortens fluorescent material.Nano fluorescent powder particles of the present invention tiny (particle diameter 30-100nm), favorable dispersity, luminescent properties are superior.To traditional green emitting phosphor long this defective time of persistence, the present invention adopts increases Mn
2+Consumption and adopt Mn
2+With Er
3+The co-activation means are overcome, to satisfy color PDP to performance demands time of persistence.
Adopt a small amount of boric acid (H in the preparation process of the present invention
3BO
3) make fusing assistant, to improve the homogeneity of preparation fluorescent material, boric acid (H
3BO
3) adding can't influence luminescent properties and other performances of fluorescent material product.The sintering process of sample (contains H at hydrogen nitrogen
210～25%, N
275～90%) finish in the atmosphere furnace.Sample behind the sintering need be handled (adopting distilled water to make dispersion agent) through ultra-sonic dispersion.
Description of drawings
Fig. 1 detects figure for the TEM of nano-phosphor of the present invention
Fig. 2 is to the mensuration curve of nano-phosphor of the present invention in PDP fluorescent material optical characteristic test system
Fig. 3 is the powder crystal diffracting spectrum of nano-phosphor of the present invention
Fig. 4 is extinction curve time of persistence of nano-phosphor of the present invention
Specific embodiments
Preparation method's embodiment 1 of the present invention the steps include:
(1) accurately weighing 7.94 restrains zinc oxide (ZnO) (analytical pure), 0.29 gram manganous carbonate (MnCO
3) (analytical pure), 0.0045 gram Erbium trioxide (Er
2O
3) (99.99%), 11.5 milligrams of tetraethoxy ((C
2H
5)
4SiO
4) (analytical pure);
(2) with zinc oxide (ZnO), manganous carbonate (MnCO
3), Erbium trioxide (Er
2O
3) mix and put into beaker;
(3) in above-mentioned beaker, add 50 milligrams of nitric acid (HNO of 1: 1
3) (analytical pure), heated and stirred is boiling extremely, and the material in the beaker is fully dissolved;
(4) add 50 ml distilled waters, and add 2 gram solubility promoter---boric acid (H
3BO
3) (analytical pure), the mixed solution in the beaker is diluted; Cooling;
(5) drip 11.5 milliliters of tetraethoxy ((C in mixed solution lentamente
2H
5)
4SiO
4), put into 60-90 ℃ water-bath device after stirring, make it peptization to transparent, spherical colloidal sol and generate;
(6) the above-mentioned colloidal sol of gained is placed 90～150 ℃ far infrared drying oven, make it to be transformed into black gray xerogel;
(7) xerogel of gained was heat-treated in 400～800 ℃ retort furnace 2 hours;
(8) after the presoma cooling with the thermal treatment gained, place 800～1200 ℃ hydrogen nitrogen (to contain H
210～25%, N
275～90%) in the atmosphere furnace, sintering is 2 hours under the competent condition of assurance reducing atmosphere, obtains fluorescent material product in early stage; Cooling;
(9) to above-mentioned fluorescent material product adding in early stage dispersion agent---water, place ultrasonic wave to carry out ultra-sonic dispersion and handle, and constantly stir;
(10) with after the filtration of the fluorescent material product behind the ultra-sonic dispersion, the loft drier of putting into 30～90 ℃ is dry, obtains required Preen nono fluorescent RE powder Zn
2-x-ySiO
4: xMn, yEr (0.01≤x≤0.15,0.0001≤y≤0.001).The performance table of the nano rare earth fluorescent material that obtains is as follows:
| The fluorescent material parameter | The fluorescent material performance |
| Chemical formula (Chemical formular) | ????Zn 1.85-1.99SiO 4:Mn 0.01-0.15Er 0.0001-0.001 |
| Granular size (grain size) | ????50nm |
| Excitation wavelength (excitation) | ????147nm |
| Predominant wavelength (λ d) | ????527nm |
| Chromaticity coordinate (CIE coordinate) | ????X＝0.2246??Y＝0.6984 |
| Peak wavelength (λ p) | ????525.7 |
| Time of persistence (τ) | ????0.983ms |
The precaution of preparation method's embodiment 1 of the present invention:
1, adds nitric acid (HNO in the step (3)
3) after, to make its boiling for some time during heating, so that the solution dissolving is fully, prevent from the recrystallize phenomenon to occur after the cooling.
2, to wait mixing solutions to cool off fully in the step (5) to put normal temperature after, again to mixed solution and dripping tetraethoxy ((C
2H
5)
4SiO
4), to prevent in the process that drips, splash taking place, reach purpose of safety.
3, in step (7) and the step (8), to sample heat-treat with sintering before, sample is not ground, form lump to prevent the sample behind the sintering.
Preparation method's embodiment 2 of the present invention the steps include:
(1) accurately weighing 7.94 restrains zinc oxide (ZnO) (analytical pure), 0.58 gram manganous carbonate (MnCO
3) (analytical pure), 0.009 gram Erbium trioxide (Er
2O
3) (99.99%), 50 milligrams of nitric acid (HNO of 1: 1
3) (analytical pure), 11.5 milligrams of tetraethoxy ((C
2H
5)
4SiO
4) (analytical pure);
(2) with zinc oxide (ZnO), manganous carbonate (MnCO
3), Erbium trioxide (Er
2O
3) mix and put into beaker;
(3) in above-mentioned beaker, add nitric acid (HNO
3), heated and stirred is boiling extremely, and the material in the beaker is fully dissolved;
(4) dilute first 2 gram boric acid are added in 50 ml distilled waters, then boric acid and distilled water solution are added in the container, the mixed solution in the beaker is diluted; Cooling;
Other step is with preparation method's embodiment 1 of the present invention.
As Fig. 1,2,3,4, the color PDP efficient green nano-phosphor Zn that is obtained in preparation method's embodiment 2 of the present invention
2-x-ySiO
4: xMn, the luminescent properties of yEr (0.01≤x≤0.15,0.0001≤y≤0.001) under vacuum ultraviolet (VUV) is superior, time of persistence is short, particle tiny (grain diameter 30-100nm, median size 50nm), good dispersion property, does not have tangible agglomeration.
Preparation method's embodiment 3 of the present invention the steps include:
(1) accurately weighing 7.94 restrains zinc oxide (ZnO) (analytical pure), 1.15 gram manganous carbonate (MnCO
3) (analytical pure), 0.0023 gram Erbium trioxide (Er
2O
3) (99.99%), 50 milligrams of nitric acid (HNO of 1: 1
3) (analytical pure), 11.5 milligrams of tetraethoxy ((C
2H
5)
4SiO
4) (analytical pure);
(2) with zinc oxide (ZnO), manganous carbonate (MnCO
3), Erbium trioxide (Er
2O
3) mix and put into beaker;
(3) in above-mentioned beaker, add nitric acid (HNO
3), heated and stirred is boiling extremely, and the material in the beaker is fully dissolved;
(4) add 50 ml distilled waters, and add 4 gram solubility promoter---boric acid (H
3BO
3) (analytical pure), the mixed solution in the beaker is diluted; Cooling;
Other step is with preparation method's embodiment 1 of the present invention.
Preparation method's embodiment 4 of the present invention: the steps include:
(1) accurately weighing 7.94 restrains zinc oxide (ZnO) (analytical pure), 0.87 gram manganous carbonate (MnCO
3) (analytical pure), 0.0045 gram Erbium trioxide (Er
2O
3) (99.99%), 50 milligrams of nitric acid (HNO of 1: 1
3) (analytical pure), 11.5 milligrams of tetraethoxy ((C
2H
5)
4SiO
4) (analytical pure);
Other step is with preparation method's embodiment 3 of the present invention.
Preparation method's embodiment 5 of the present invention: the steps include:
(1) accurately weighing 8.73 restrains zinc oxide (ZnO) (analytical pure), 1.27 gram manganous carbonate (MnCO
3) (analytical pure), 0.009 gram Erbium trioxide (Er
2O
3) (99.99%), 5 gram boric acid (H
3BO
3) (analytical pure), dissolve with 50 ml distilled waters;
Other step is with preparation method's embodiment 1 of the present invention.
Preparation method's embodiment 6 of the present invention: the steps include:
(1) accurately weighing 8.25 restrains zinc hydroxide (Zn (OH)
2) (analytical pure), 0.58 gram manganous carbonate (MnCO
3) (analytical pure), 0.009 gram Erbium trioxide (Er
2O
3) (99.99%), 50 milligrams of nitric acid (HNO of 1: 1
3) (analytical pure), 11.5 milligrams of tetraethoxy ((C
2H
5)
4SiO
4) (analytical pure);
(2) with zinc hydroxide (Zn (OH)
2), manganous carbonate (MnCO
3), Erbium trioxide (Er
2O
3) mix and put into beaker;
(3) in above-mentioned beaker, add nitric acid (HNO
3), heated and stirred is boiling extremely, and the material in the beaker is fully dissolved;
(4) dilute first 4 gram boric acid are added in 50 ml distilled waters, then boric acid and distilled water solution are added in the container, the mixed solution in the beaker is diluted; Cooling;
Other step is with preparation method's embodiment 1 of the present invention.
Preparation method's embodiment 7 of the present invention: the steps include:
(1) accurately weighing 8.42 restrains zinc hydroxide (Zn (OH)
2) (analytical pure), 2.06 gram manganous nitrate (Mn (NO
3)
2) (analytical pure), 0.018 gram Erbium trioxide (Er
2O
3) (99.99%), 50 milligrams of nitric acid (HNO of 1: 1
3) (analytical pure), 11.5 milligrams of tetraethoxy ((C
2H
5)
4SiO
4) (analytical pure);
(2) with zinc hydroxide (Zn (OH)
2), manganous nitrate (Mn (NO
3)
2), Erbium trioxide (Er
2O
3) mix and put into beaker;
(3) in above-mentioned beaker, add nitric acid (HNO
3), heated and stirred is boiling extremely, and the material in the beaker is fully dissolved;
(4) dilute first 2 gram boric acid are added in 50 ml distilled waters, then boric acid and distilled water solution are added in the container, the mixed solution in the beaker is diluted; Cooling;
Other step is with preparation method's embodiment 1 of the present invention.
Preparation method's embodiment 8 of the present invention: the steps include:
(1) accurately weighing 7.94 restrains zinc oxide (ZnO) (analytical pure), 2.63 gram manganous nitrate (Mn (NO
3)
2) (analytical pure), 0.0015 gram Erbium trioxide (Er
2O
3) (99.99%), 50 milligrams of nitric acid (HNO of 1: 1
3) (analytical pure), 11.5 milligrams of tetraethoxy ((C
2H
5)
4SiO
4) (analytical pure);
(2) with zinc oxide (ZnO), manganous nitrate (Mn (NO
3)
2), Erbium trioxide (Er
2O
3) mix and put into beaker;
(3) in above-mentioned beaker, add nitric acid (HNO
3), heated and stirred is boiling extremely, and the material in the beaker is fully dissolved;
(4) add 50 ml distilled waters, and add 3 gram solubility promoter---boric acid (H
3BO
3) (analytical pure), the mixed solution in the beaker is diluted; Cooling;
Other step is with preparation method's embodiment 1 of the present invention.
With the resulting fluorescent material product of above embodiment, under VUV and shortwave UV light and electron-beam excitation, launch strong green glow, emission peak is 530nm.The time of persistence of sample is short, particle is tiny (median size 50nm), favorable dispersity, and its performance meets color PDP fully to the fluorescent material performance demands.
Claims (8)
1, a kind of nano-phosphor is characterized in that: it is a compound, and its chemical formula consists of:
Zn
2-x-ySiO
4:xMn，yEr
Wherein: 0.01≤x≤0.15,0.0001≤y≤0.001;
Its grain diameter 30-100nm.
2, prepare the method for nano-phosphor according to claim 1, it is characterized in that: its step comprises:
(1) presses soluble zinc salt or zinc oxide/tetraethoxy=1.85～1.99: 1, soluble manganese salt/Erbium trioxide=20～3000: 1, soluble zinc salt or zinc oxide/soluble manganese salt=5～40: 1 mole ratio, accurately weighing soluble zinc salt or zinc oxide, tetraethoxy, soluble manganese salt, Erbium trioxide;
(2) soluble zinc salt or zinc oxide, soluble manganese salt, Erbium trioxide are mixed put into container;
(3) add 1: 1 nitric acid in said vesse, heated and stirred is to boiling, and the material in the container is fully dissolved; Per 1 gram soluble zinc salt or zinc oxide, soluble manganese salt, Erbium trioxide solid total mass add 4～10 milliliters of nitric acid of 1: 1.
(4) add distilled water, and add solubility promoter---boric acid, the mixed solution in the container is diluted;
(5) in mixed solution, drip tetraethoxy, put into 60-90 ℃ water-bath device after stirring, make it peptization to transparent, spherical colloidal sol and generate;
(6) the above-mentioned colloidal sol of gained is placed 90～150 ℃ far infrared drying oven, make it to be transformed into xerogel;
(7) xerogel of gained was heat-treated in 400～800 ℃ retort furnace 1～4 hour;
(8) after the presoma cooling with the thermal treatment gained, place 800～1200 ℃ hydrogen and nitrogen gas atmosphere stove, sintering is 1～4 hour under the competent condition of assurance reducing atmosphere, obtains fluorescent material product in early stage; Contain H in the hydrogen and nitrogen gas atmosphere stove
210～25%, N
275～90%;
(9) to above-mentioned fluorescent material product adding in early stage dispersion agent---water, place ultrasonic wave to carry out ultra-sonic dispersion and handle;
(10) with after the filtration of the fluorescent material product behind the ultra-sonic dispersion, the loft drier of putting into 30～90 ℃ is dry, obtains required product.
3, preparation method as claimed in claim 2 is characterized in that: in the step (4), distilled water is diluted to 150～300% of original volume with mixed solution; The quality that adds boric acid is 1%～15% of soluble zinc salt or zinc oxide, soluble manganese salt, an Erbium trioxide solid total mass.
4, preparation method as claimed in claim 2 is characterized in that: when in the step (4) mixed solution being diluted, boric acid is added in the distilled water dilutes earlier, then with in boric acid and the distilled water solution adding container; The quality of boric acid is 1%～15% of soluble zinc salt or zinc oxide, soluble manganese salt, an Erbium trioxide solid total mass; The mass ratio of boric acid and distilled water is 1: 5～1: 15.
5, as claim 2 or 3 or 4 described preparation methods, it is characterized in that: the rate of addition of tetraethoxy is controlled at 5～10 ml/min.
6, as claim 2 or 3 or 4 described preparation methods, it is characterized in that: in the step (9), the add-on of water is 2～10 times of adding fluorescent material quality, and the time that places ultrasonic wave to carry out the ultra-sonic dispersion processing is 1-5 hour;
7, as claim 2 or 3 or 4 described preparation methods, it is characterized in that: soluble zinc salt is a zinc hydroxide.
8, as claim 2 or 3 or 4 described preparation methods, it is characterized in that: soluble manganese salt is manganous carbonate or manganous nitrate.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310111208 CN1285704C (en) | 2003-10-08 | 2003-10-08 | Nano fluorescent powder and preparing method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310111208 CN1285704C (en) | 2003-10-08 | 2003-10-08 | Nano fluorescent powder and preparing method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1528858A true CN1528858A (en) | 2004-09-15 |
| CN1285704C CN1285704C (en) | 2006-11-22 |
Family
ID=34304732
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
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| Country | Link |
|---|---|
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1325601C (en) * | 2005-02-21 | 2007-07-11 | 东南大学 | Method for preparing small grain size manganese zinc silicate green fluorescent powder |
| CN104393157A (en) * | 2014-11-24 | 2015-03-04 | 上海祥羚光电科技发展有限公司 | Fluorescent plastic master batch production and application for LED (Light Emitting Diode) white light secondary light conversion |
| CN111978956A (en) * | 2020-08-26 | 2020-11-24 | 广东工业大学 | Orange light long afterglow fluorescent powder and preparation method thereof |
-
2003
- 2003-10-08 CN CN 200310111208 patent/CN1285704C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1325601C (en) * | 2005-02-21 | 2007-07-11 | 东南大学 | Method for preparing small grain size manganese zinc silicate green fluorescent powder |
| CN104393157A (en) * | 2014-11-24 | 2015-03-04 | 上海祥羚光电科技发展有限公司 | Fluorescent plastic master batch production and application for LED (Light Emitting Diode) white light secondary light conversion |
| CN111978956A (en) * | 2020-08-26 | 2020-11-24 | 广东工业大学 | Orange light long afterglow fluorescent powder and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1285704C (en) | 2006-11-22 |
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