CN1267526C - Preparation process of vacuum ultraviolet borate fluorescent material - Google Patents
Preparation process of vacuum ultraviolet borate fluorescent material Download PDFInfo
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- CN1267526C CN1267526C CN 200410025945 CN200410025945A CN1267526C CN 1267526 C CN1267526 C CN 1267526C CN 200410025945 CN200410025945 CN 200410025945 CN 200410025945 A CN200410025945 A CN 200410025945A CN 1267526 C CN1267526 C CN 1267526C
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Abstract
The present invention discloses a hydrothermal preparation method of vacuum ultraviolet borate luminescent materials, wherein the chemical formula of the vacuum ultraviolet borate luminescent materials is Y<1-x-y>Eu<x>Gd<y>BO3, the x is at least 0.05 and at most 0.3, and the y is at leat 0.01 and at most 0.6. Yttrium nitrate, gadolinium nitrate, europium nitrate and an organic reagent, such as tributyl borate are caused to react on condition that acid or base is used as a hydrolyst by a hydrothermal method. Compared with the prior art, the present invention has the advantages of low reaction temperature of the preparation method, simple operation and controllable granularity and topography of the vacuum ultraviolet borate luminescent materials. The spherical fluorescent powder of the present invention has high coating property, high bulk density of the fluorescent powder can be obtained, and vacuum-ultraviolet light can be preferably absorbed by the fluorescent powder. In addition, the luminous efficiency of the fluorescent powder under the excitation of vacuum ultraviolet light can be improved, so the luminance of luminescent screens is favorable to be improved, and the requirement for high luminance of plasma displays can be preferably satisfied.
Description
Technical field
The present invention relates to a kind of preparation method of vacuum ultraviolet (VUV) borate fluorescent material, more definite say that involved in the present invention is (Y, Gd) BO
3: Eu Preparation of Fluorescent Material method.
Background technology
Mix Eu
3+(Y, Gd) BO
3Be a kind of red fluorescence powder of excellent performance, this fluorescent material has good absorption in the UV and VUV district, and exciting down at 147nm has higher luminous efficiency, is widely used at present in the plasma display (PDP).(Y, Gd) BO in the prior art
3: Eu generally is synthetic with solid phase method, and its temperature of reaction is 1100 ℃～1400 ℃.Because B when temperature is higher than 800 ℃
2O
3Can volatilize, add excessive H
3BO
3Perhaps B
2O
3Loss with B in the compensation high-temperature calcination process.In addition, adopt solid phase method synthetic (Y, Gd) BO
3: the sintering phenomenon that can produce fluorescent material during Eu because of high-temperature calcination.For the fluorescent material that obtains granularity and be fit to, be evenly distributed just must carry out milled processed to the fluorescent material of preparation, but this can reduce the brightness of fluorescent material.In recent years, many new synthetic methods have appearred, sol-gel method for example, microwave method etc.RaoRavilisetty has at first synthesized (Y, Gd) BO with sol-gel method
3: Eu fluorescent material.But sol-gel method preparation (Y, Gd) BO
3: Eu must could obtain single-phasely heat-treating more than 900 ℃, and its essence also is solid state reaction, can have all deficiencies of solid-phase synthesis equally.Utilize microwave method to synthesize (Y, Gd) BO
3: Eu fluorescent material, because initial feed such as Y
2O
3, Eu
2O
3Deng being the oxide compound that seldom absorbs microwave, therefore need cover one deck microwave absorbing medium outside raw material could effectively utilize microwave to react.Therefore it is all lower to prepare the purity and the luminous efficiency of fluorescent material with microwave method.And above method all is limited to the control of pattern.
Hydrothermal method is a kind of emerging method of Recent study inorganic materials synthetic, this method is the dissolvable oxides of metal and non-metallic element or salt to be dissolved in reaction medium (water or other liquid) be placed in the pressurized vessel of sealing reacting by heating at a certain temperature, can obtain product.Advantages such as this method has that reaction conditions is gentle relatively, the reaction times is short, process is simple, synthesis temperature is low, product pattern and controllable granularity, and the powder of Hydrothermal Preparation do not need to grind, do not have reunite, good dispersity.One of the present inventor Wang Yuhua is at " GdBO
3: Eu Phosphor Particles with Uniform Size, PlateMorphology, and Non-Aggregation " (Yuhua Wang, et al.; Chem.Lett., 2001 (3): 206-207) disclose first in the literary composition with the synthetic even-grained sheet GdBO of hydrothermal method
3: the method for Eu fluorescent material.This method is to carry out evaporate to dryness after gadolinium sesquioxide, europium sesquioxide and boron trioxide are dissolved in nitric acid, then the residue behind the evaporate to dryness is placed the small-sized stainless steel cauldron of teflon lined, adds distilled water and reacts the flaky GdBO of back acquisition at 300 ℃
3: Eu fluorescent material.But platy particle luminous efficiency under 147nm excites is very low, has only 50% of solid state reaction gained sample.
Discover the luminous efficiency height of spherical phosphor, can better absorb vacuum-ultraviolet light, and spheric fluorescent material coating is good, can obtain high tap density, for PDP fluorescent material, the optimum size scope is between the 3-5 micron, requirement is evenly distributed and does not have reunion ([1] R.P.Rao and D.J.Devine, Present Status of PDP Phosphors, p.152, International Conference onLuminescence and Optical Spectroscopy of Condensed Matter, Osaka, Japan (1999) .[2] Y.C.Kang, I.W.Lenggoro, K.Okuyama and S.B.Park, J.Electrochem.Soc.1999.146 (3:1227.).But can't obtain the spheric particle in the prior art.
Summary of the invention
The invention provides and a kind ofly can control vacuum ultraviolet (VUV) borate fluorescent material (Y
1-x-yEu
xGd
y) BO
3The granularity of (0.05≤x≤0.3,0.01≤y≤0.6) and the hydrothermal preparing process of pattern.A kind of sphere (Y, Gd) BO of size-grade distribution homogeneous particularly are provided
3: Eu Preparation of Fluorescent Material method.
Method of the present invention is that Yttrium trinitrate, Gadolinium trinitrate, europium nitrate and boric acid ester water and ethanolic soln are dissolved, the hydrolyst that adds acid or bases then, the pH value scope that makes solution is 5～6, mixing solutions is transferred in the small-sized stainless steel cauldron of teflon lined, be incubated 6 hours down at 240～280 ℃, with dehydrated alcohol and distilled water wash, carry out filtration drying again and handle after reaction is finished, obtain spheric (Y, Gd) BO at last
3: Eu fluorescent material.By kind to water in the reaction system and alcoholic acid ratio, hydrolyst, and the kind of the different hydrolysts that added and to the acidity control of system, can realize control to product pattern and granularity.
The source of yttrium of the present invention, gadolinium and europium also can be the oxide compound of yttrium, gadolinium and europium, it is obtained the salt of yttrium, gadolinium and europium with nitric acid treatment again.
Boric acid ester of the present invention is trimethyl borate or tributyl borate.
Water and alcoholic acid volume ratio can obtain monophasic product at 1: 1～1: 3.5 o'clock among the present invention, less than occurring impurity at 1: 1, and formed non-crystalline state greater than 1: 3.5 o'clock, as shown in Figure 2.Water and alcoholic acid optimum volume ratio are 1: 2 among the present invention.
The hydrolyst that is added in the reaction system of the present invention can be acid or alkali.When adopting acid, preferably adopt nitric acid or boric acid as hydrolyst.Preferably use ammoniacal liquor when adopting alkali, because adopt other kind acid or alkali all will make foreign matter content rising in the product.Relevant studies show that, when adopting nitric acid to be hydrolyst, the fluorescent material of gained is spherical, and particle surface is comparatively coarse, if during as hydrolyst, can obtain ganoid spherical phosphor with boric acid, but the possible skewness of its granularity.If it is hydrolyst that the present invention adopts ammonia, not only can obtain ganoid spherical phosphor, and the size-grade distribution of gained powder is more even.
The range of reaction temperature of the best of the present invention is 240～280 ℃.(below 180 ℃) its crystallization effect is relatively poor when low as temperature of reaction, though can promote crystallization when temperature of reaction is too high, preferred orientation takes place easily.Therefore, the range of reaction temperature of the best of the present invention is 240～280 ℃.
Growth has certain influence to solution pH value of the present invention to crystalline, and pH value not only influences the solubleness of solute, and might change the structure of growth unit, finally influences crystalline structure, shape and size.1≤PH among the present invention＜5 o'clock easily produce non-globular particle, and can obtain varigrained spheroidal particle when pH is 5≤PH≤6.Therefore the PH in the present invention's reaction should be good 5～6.
The present invention compared with prior art has following advantage:
1, temperature of reaction is low, and preparation cost is low, and the purity height of products therefrom, good dispersity, and no agglomeration also need not to carry out the milled processed in later stage again;
2, the products therefrom form is controlled, the spherical product that the granularity that is easy to get is fit to (being about 3～5 microns), is evenly distributed, and the while also can form the product of the uneven spherical-like morphology of granularity, to adapt to the needs of particular application;
3, (Y, Gd) BO for preparing with method of the present invention
3: Eu fluorescent material, its activator (Eu
3+) quenching concentration be 20%, and the sample of solid state reaction gained has only 10%, luminescence center of this explanation products therefrom of the present invention is more than the luminescence center of solid state reaction, thereby luminescent properties is better than solid state reaction gained sample;
4, method preparation (Y, Gd) BO of the present invention
3: during Eu, reactant is to mix on atom or molecular level, therefore can make activator (Eu
3+) more be evenly distributed in the lattice dot matrix;
5, method preparation (Y, Gd) BO of the present invention
3: the raw material of Eu is accurately to take by weighing according to stoichiometric ratio, and B in the solid state reaction
2O
3Or H
3BO
3Must be excessive 5%～15%, so the defective of product can increase, this can reduce the luminous intensity of fluorescent material;
6, the sample of the strength ratio solid state reaction preparation of the strong emission peak of the spherical fluorescent material of gained of the present invention under 254nm excites exceeds more than 2 times, excites down the sample of the strength ratio solid state reaction preparation of strong emission peak to exceed more than 10% at 147nm.
Description of drawings
Accompanying drawing 1 is the X diffractogram of the present invention and relevant contrast experiment's products therefrom.
Accompanying drawing 2 for be among the present invention when water and ethanol different ratios to the figure that influences of product.
Accompanying drawing 3 is for being raw material with Yttrium trinitrate etc. with tributyl borate, with boric acid as hydrolyst, the sem photograph of products therefrom.
Accompanying drawing 4 is for being raw material with Yttrium trinitrate etc. with tributyl borate, with nitric acid as hydrolyst, the sem photograph of products therefrom.
Accompanying drawing 5 is for being raw material with Yttrium trinitrate etc. with tributyl borate, with ammoniacal liquor as hydrolyst, the sem photograph of products therefrom.
Accompanying drawing 6 is the sem photograph of disclosed hydrothermal method products therefrom.
Accompanying drawing 7 is the sem photograph of solid state reaction products therefrom.
Accompanying drawing 8 is products therefrom exciting light spectrogram (E of the present invention
m=591nm).
Accompanying drawing 9 is the emmission spectrum figure (E of products therefrom of the present invention
x=254nm).
Embodiment
Several embodiments of the present invention below are provided.
Initial feed of the present invention mainly is made up of the raw material that Y element, Eu element, Gd element, B element are provided.Y is provided, Eu, the initial feed of Gd element has been selected following two kinds for use: oxide compound, nitrate.When adopting oxide compound, should in advance itself and dilute nitric acid reaction be generated nitrate.The raw material that the B element is provided is a tributyl borate.Y in each embodiment, Eu, after the raw material of Gd element and B element mixes by stoichiometric ratio, join in the water and ethanolic soln (volume ratio is 1: 2) as reaction solvent, the pH value that adds the hydrolyst regulator solution again is 5～6, mixing solutions is transferred in the small-sized stainless steel cauldron of teflon lined, be incubated 6 hours down at 240～280 ℃, after reaction finishes, furnace cooling is to room temperature, wash with dehydrated alcohol and distilled water respectively, product 100 ℃ of dryings, promptly gets the purpose product after filtering.
In order to compare with prior art, adopted in solid reaction process and the prior art disclosed Hydrothermal Preparation respectively (Y, Gd) BO
3: Eu.When adopting solid phase method to prepare, its initial feed is Y
2O
3, Gd
2O
3, H
3BO
3, Eu
2O
3, press the accurate weighing of stoicheiometry (H wherein
3BO
3Excessive 5%～15%) the back mixed grinding is even, 500 ℃ of heating 2.5 hours, promptly gets required sample in 2 hours in 1100 ℃ of sintering behind the taking-up regrinding.Adopt the disclosed Hydrothermal Preparation of prior art (Y, Gd) BO
3: during Eu, raw materials used is Yttrium trinitrate, europium nitrate, Gadolinium trinitrate and boric acid, and reaction solvent is a distilled water, does not use other material as hydrolyst.
Products therefrom has been analyzed the thing phase with Japanese Rigaku D/MAX-2400 type X-ray diffractometer of science in the embodiments of the invention, with the pattern of JSM-5600LV rough vacuum sem observation sample, at room temperature record burst of ultraviolel spectrum and emmission spectrum with the F-4500 of Hitachi type fluorescence spectrophotometer.The characteristics of luminescence under vacuum ultraviolet-excited is to record and proofread and correct with sodium salicylate (Sodium Benzoate) with ARC Model VM-502 type vacuum monochromator.
Embodiment 1
Initial feed: Yttrium trinitrate, Gadolinium trinitrate, europium nitrate, tributyl borate; Solvent: distilled water: ethanol=1: 2 (volume ratio); Catalyzer: be boric acid.
Preparation process: Yttrium trinitrate, Gadolinium trinitrate, europium nitrate, tributyl borate are taken by weighing by stoichiometric ratio, join then in water and the alcoholic acid mixing solutions (water: the ethanol volume ratio is 1: 2), overall solution volume is 18 milliliters.Under ultrasonic dispersing, dripping rare nitric acid, to make solution PH be 5～6.This solution moved into to be had in the small-sized stainless steel cauldron of teflon lined, and 260 ℃ of insulations 6 hours, after reaction finished, furnace cooling was used dehydrated alcohol and distilled water wash respectively to room temperature, filters at last and 100 ℃ of dryings.Promptly obtain spheric (Y
1-x-yEu
xGd
y) BO
3(0.05≤x≤0.3,0.01≤y≤0.6) fluorescent material.
The present embodiment mesoboric acid be hydrolyst also be the reaction initial feed.
Measurement result: X-ray diffraction analysis shows that products therefrom is single-phase, sees curve a in the accompanying drawing 1.Scanning electron microscope analysis shows that resulting powder is spherical, and smooth surface is seen accompanying drawing 3.As seen from the figure, its size-grade distribution is inhomogeneous.
Embodiment 2
Initial feed: Yttrium trinitrate, europium nitrate, Gadolinium trinitrate, tributyl borate; Solvent: distilled water: ethanol=1: 2; Catalyzer: be nitric acid.
Preparation process: Yttrium trinitrate, europium nitrate, Gadolinium trinitrate and tributyl borate are taken by weighing by stoichiometric ratio, join then in water and the alcoholic acid mixing solutions (water: the ethanol volume ratio is 1: 2), overall solution volume is 18 milliliters.Under ultrasonic dispersing, dripping rare nitric acid, to make solution PH be 5 ~ 6.Mixing solutions moved into to be had in the small-sized stainless steel cauldron of teflon lined, and 260 ℃ of insulations 6 hours, after reaction finished, furnace cooling was used dehydrated alcohol and distilled water wash respectively to room temperature, filters at last and 100 ℃ of dryings.Promptly obtain spheric (Y
1-x-yEu
xGd
y) BO
3(0.05≤x≤0.3,0.01≤y≤0.6) fluorescent material.
Nitric acid must adopt rare nitric acid in the present embodiment.
Measurement result: X-ray diffraction analysis shows that the gained powder is single-phase, sees curve b in the accompanying drawing 1.Scanning electron microscope analysis shows that resulting powder is spherical, sees accompanying drawing 4.By accompanying drawing as seen, comparatively coarse at its particle surface, at particle surface the corrosive vestige is arranged.
Embodiment 3
Initial feed: Yttrium trinitrate, europium nitrate, Gadolinium trinitrate, tributyl borate; Solvent: distilled water: ethanol=1: 2 (volume ratio); Catalyzer: be ammoniacal liquor.
Preparation process: take by weighing with Yttrium trinitrate, europium nitrate, Gadolinium trinitrate and tributyl borate with by stoichiometric ratio, join then in water and the alcoholic acid mixing solutions (water: the ethanol volume ratio is 1: 2), overall solution volume is 18 milliliters.Under ultrasonic dispersing, form colloidal sol at mixed solution and dripping ammoniacal liquor.This colloidal sol moved into to be had in the small-sized stainless steel cauldron of teflon lined, and 260 ℃ of insulations 6 hours, after reaction finished, furnace cooling was used dehydrated alcohol and distilled water wash respectively to room temperature, filters at last and 100 ℃ of dryings, promptly obtains spheric (Y
1-x-yEu
xGd
y) BO
3(0.05≤x≤0.3,0.01≤y≤0.6) fluorescent material.
The rare more easy more spherical phosphor that obtains of collosol concentration in the present embodiment.
Measurement result: X-ray diffraction analysis shows that the gained powder is single-phase, sees curve c in the accompanying drawing 1.Scanning electron microscope analysis shows that resulting powder is a uniform spherical, referring to accompanying drawing 3.By accompanying drawing as seen, present embodiment products therefrom smooth surface, size of particles is even, and its size is about the 2-3.5 micron.Excite down at 254nm, during x=0.2, its strongest emission peak intensity is 2 times of solid state reaction gained sample.Excite down at 147nm, luminous strength ratio Japan changes into (Y, Gd) BO that stock company produces
3: the commercial powder of Eu (KX-504A) has improved 10%.
The experiment that compares with the present invention is:
Comparative Examples 1
Initial feed: yttrium oxide etc., boric acid; Solvent: distilled water.
Preparation process: yttrium oxide, europium sesquioxide, gadolinium sesquioxide and boron oxide are taken by weighing by stoichiometric ratio, add evaporate to dryness behind the dilute nitric acid dissolution, adding distilled water in the resistates behind evaporate to dryness, to make overall solution volume be 18 milliliters.This mixing solutions is changed in the small-sized stainless steel cauldron of teflon lined.300 ℃ of insulations 3 hours, after reaction finished, furnace cooling use distilled water wash to room temperature, filtration at last and 100 ℃ of dryings.Flaky (Y, Gd) BO have promptly been obtained
3: the Eu powder.
Measurement result: X-ray diffraction analysis shows that the gained powder is single-phase, consistent with bibliographical information.Scanning electron microscope analysis shows that resultant particle is uniform sheet, referring to accompanying drawing 6.
Comparative Examples 2
Adopt solid reaction process to prepare (Y, Gd) BO
3: Eu, initial feed is yttrium oxide, gadolinium sesquioxide, boric acid, europium sesquioxide, by the accurate weighing of stoichiometric ratio (H wherein
3BO
3Excessive 5%～15%) the back mixed grinding is even, 500 ℃ of heating 2.5 hours, promptly obtains sample in 2 hours in 1100 ℃ of sintering behind the taking-up regrinding.
Measurement result: X-ray diffraction analysis shows that the gained powder is single-phase, consistent with bibliographical information.Scanning electron microscope analysis shows that resultant particle is irregular, sees accompanying drawing 7.Excitation spectrum is seen the curve b of accompanying drawing 8.Emmission spectrum is seen the curve b of accompanying drawing 9.
Claims (8)
1, a kind of (Y
1-x-yEu
xGd
y) BO
3(0.05≤x≤0.3,0.01≤y≤0.6) Preparation of Fluorescent Material method, it is characterized in that Yttrium trinitrate, Gadolinium trinitrate, europium nitrate and boric acid ester are dissolved in water and the ethanolic soln, in system, add acid or ammoniacal liquor hydrolyst, system is heated to 200～300 ℃ reacts, the pH value of system with dehydrated alcohol and distilled water wash, carries out filtration drying again and handles after reaction is finished smaller or equal to 6 during reaction.
2, preparation method according to claim 1 is characterized in that described boric acid ester is trimethyl borate or tributyl borate.
3, preparation method according to claim 2 is characterized in that the system temperature of reaction is 240～280 ℃.
4, preparation method according to claim 3, the pH value of the system when it is characterized in that reacting is 5～6.
5, preparation method according to claim 4 is characterized in that water and ethanol volume ratio are 1: 1～1: 3.5 in the used solvent.
6, preparation method according to claim 5 is characterized in that water and ethanol volume ratio are 1: 2 in the used solvent.
7, according to described arbitrary preparation method among the claim 1 to 6, the hydrolyst that it is characterized in that in the system being added is nitric acid or boric acid.
8, according to described arbitrary preparation method among the claim 1 to 6, the hydrolyst that it is characterized in that in the system being added is an ammoniacal liquor.
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|---|---|---|---|
| CN 200410025945 CN1267526C (en) | 2004-02-25 | 2004-02-25 | Preparation process of vacuum ultraviolet borate fluorescent material |
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|---|---|---|---|
| CN 200410025945 CN1267526C (en) | 2004-02-25 | 2004-02-25 | Preparation process of vacuum ultraviolet borate fluorescent material |
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| CN1267526C true CN1267526C (en) | 2006-08-02 |
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| CN102442778B (en) * | 2010-09-30 | 2014-06-04 | 惠州晶宝光电科技有限公司 | Fluorescent glass and preparation method and application thereof |
| CN106590654A (en) * | 2016-12-08 | 2017-04-26 | 兰州理工大学 | Method for synthesizing composite light-emitting material high in ultraviolet-visible absorption efficiency |
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