CN105176526A - Preparation method of low-voltage and high-brightness orange red zinc-sulfate-based fluorescent material - Google Patents
Preparation method of low-voltage and high-brightness orange red zinc-sulfate-based fluorescent material Download PDFInfo
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- CN105176526A CN105176526A CN201510707191.XA CN201510707191A CN105176526A CN 105176526 A CN105176526 A CN 105176526A CN 201510707191 A CN201510707191 A CN 201510707191A CN 105176526 A CN105176526 A CN 105176526A
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Abstract
A preparation method of a low-voltage and high-brightness orange red zinc-sulfate-based fluorescent material is characterized by including the steps of evenly mixing fluorescent-grade zinc sulfate doped main activator manganese ions, auxiliary activator and fluxing agents, adding the mixture in a double-layer aluminum oxide or quartz crucible, conducting sintering at the temperature of 1150-1200 DEG C for 2-3 hours, conducting natural cooling at the room temperature, and conducting screening, water washing, drying and surface wrapping, a stannic oxide nanometer material is used for surface wrapping, and orange red light is emitted under the alternating voltage of 36 V.
Description
Technical field
The invention belongs to the manufacture field of fluorescent material in luminescence display illumination, be namely main substance with zinc sulphide, copper, manganese, selenium, cadmium, zinc is the fluorescent material of activator.The fluorescent material manufactured may be used for AC electroluminescence, vacuum fluorescent display (VFD), Field Emission Display (FED) and cathode-ray tube (CRT).
Background technology
Sulphide fluorescent material is the class luminescent material comparatively early found, is particularly that the fluorescent material of matrix is as blue colour fluorescent powder (ZnS:Ag, Cl with ZnS; ZnS:Ag, Al; ZnS:Zn), green emitting phosphor (ZnS:Cu, Al), yellow fluorescent powder (ZnS:Au, Al), orange fluorescent powder (ZnS:Cu, Mn), emitting red light (CdZnS:Cu, CdZnSe:Ag) they are still widely used in negative ray colour picture tube (CRT) so far, vacuum fluorescence display charactron (VFD), electroluminescent display board (EL) and field emitting display panel (FED), current vacuum fluorescence display charactron all uses above-mentioned fluorescent material.Wherein orange ZnS:Mn material is prepared into quantum dot, electroluminescent has extensive announcement in the patent of various countries.
Chinese patent 03112201.9, 02138536.X, the preparation methods disclosing this kind of luminescent material such as 871080869, comprise the preparation of the mixing solutions of activator and solubility promoter, activator is cupric chloride, copper sulfate, cupric bromide, one or more of Manganous chloride tetrahydrate, solubility promoter is sodium-chlor, magnesium chloride, one or more of bariumchloride, mixing solutions and Fluorescence Grade zinc sulphide powder mix, add sulphur powder again, with 1100-1150 DEG C of constant temperature 2.5-3.5 hour in alumina crucible, naturally cooling to luminescent material, carrying out double sintering, the product of surface copper-clad.But this method products obtained therefrom granularity is comparatively large, affects the range of application of luminescent powder, is not suitable with the market requirement of current most of information products indicating meters, and the stink damp cognition that experimentation uses impacts environment.Chinese patent 200710037164.1 is also had to disclose a kind of preparation method of zinc sulfide phosphor through reprocessing and supersound process, processing uses high-energy ball milling or isostatic pressed method, its technical process is too complicated, and processing condition require comparatively strict, are unfavorable for batch production.
The object of this invention is to provide the preparation method of the orange red zinc sulfide-based fluorescent material of a kind of low-voltage high-brightness; and the method more environmental protection cleaner than traditional method; do not adopt dithiocarbonic anhydride; toxic gases such as hydrogen sulfide but only add sulphur as atmosphere protection in whole experimentation, produce orange red luminescence simultaneously.
Summary of the invention
The invention provides the preparation method of the orange red zinc sulfide-based fluorescent material of a kind of low-voltage high-brightness, it is characterized in that: Fluorescence Grade zinc sulphide doping dominant activator mn ion, auxiliary activator, fusing assistant are mixed, load in double layer aluminium oxide or quartz crucible, fire 2-3 hour for 1150-1200 DEG C, then at room temperature naturally cooling, then screen, washing, oven dry, Surface coating; Surface coating uses tin dioxide nanometer material, and it launches orange red luminescence under voltage of alternating current 36V.
Mixed with dopant ion by cooled material in the present invention, load in aluminum oxide or quartz crucible and carry out double sintering, fire 2-3 hour, be cooled to room temperature for 600-800 DEG C, finally screened by the material after burning, namely washing, oven dry obtain finished product.
Dopant ion described in the present invention is copper, manganese, selenium, cadmium; Tin dioxide nanometer material uses stanniferous acidic solution, utilizes hydrothermal method to prepare, and mixes, dries with zinc sulphide matrix fluorescent material.In the present invention, the surface treatment of tin dioxide nanometer material uses hydrochloric acid to adjust pH value weakly acidic pH, and the long wave that can affect electroluminescent spectrum moves, and makes work exchange voltage be down to safety range under 36V simultaneously.
Fusing assistant described in the present invention is that muriate is as one or more in sodium-chlor, magnesium chloride, ammonium chloride etc. or bromide, as one or more in Sodium Bromide, magnesium bromide, brometo de amonio etc., wherein bromide can be that emmission spectrum length is moved, and improves luminous intensity and life-span.
The compound of the copper of the dopant ion described in the present invention is cupric chloride, cupric bromide, copper sulfate; The compound of zinc is zinc oxide, zinc selenide; The compound of manganese is Manganous chloride tetrahydrate, manganous nitrate, Manganese dibromide; Selenium compound is zinc selenide, cadmium selenide, and the compound of cadmium is Cadmium Sulfide.
Washing methods described in the present invention is for first to wash, and then pickling, then be washed to neutrality, subsequently alkali cleaning, is finally washed to neutrality.Alkali lye described in the present invention is volatile salt, deionized water, hydrogen peroxide, the mixing solutions of ammoniacal liquor.It is characterized in that in the present invention: Surface coating uses tin dioxide nanometer material, use the organic compound material of tin, prepared by hydrothermal method, tin dioxide nanometer material uses hydrochloric acid adjustment pH value weakly acidic pH, emmission spectrum is 600nm, the luminescence feature spectrum main peak of usual mn ion is shown as 585nm orange luminescence, and spectrum is shown as the orange red luminescence of 600nm after method of the present invention and surface treatment, make material can be widely used in the luminescence of white and display device, compensate for the deficiency of red component luminescence, reduce use voltage.
Accompanying drawing explanation
Fig. 1 is the made ZnS:Cu of embodiment 1, Mn fluorescent powder grain size.
Fig. 2 is the made ZnS:Cu of embodiment 1, Mn fluorescent powder grain surface topography.
specific implementation method
The preparation method of the orange red zinc sulfide-based fluorescent material of a kind of low-voltage high-brightness of the present invention, it is characterized in that: Fluorescence Grade zinc sulphide doping dominant activator mn ion, auxiliary activator, fusing assistant are mixed, load in double layer aluminium oxide or quartz crucible, fire 2-3 hour for 1150-1200 DEG C, then at room temperature naturally cooling, then screen, washing, oven dry, Surface coating; Surface coating uses tin dioxide nanometer material, and use hydrochloric acid adjustment pH value weakly acidic pH, it launches orange red luminescence under voltage of alternating current 36V.
The manufacture of zinc sulfide-based fluorescent material generally has two kinds of methods, and it is fusing assistant that first method employing adds halogenide in the feed, then adds sulphur mixing, and uses carbon dust covering surfaces, fires in atmosphere and forms; Second method adopts to add fusing assistant in the feed, fires and form in dithiocarbonic anhydride or hydrogen sulfide atmosphere; First method utilizes sulphur and carbon dust to produce carbon disulfide gas to promote in pyroreaction and react, and these two kinds of methods all produce dithiocarbonic anhydride or hydrogen sulfide toxic gas, to environment.The object of this invention is to provide the preparation method of the oligosaprobic orange zinc sulfide-based fluorescent material of a kind of high brightness; and the method more environmental protection cleaner than traditional method; do not adopt dithiocarbonic anhydride, toxic gases such as hydrogen sulfide but only add sulphur as atmosphere protection in whole experimentation.The technical scheme of technical solution problem of the present invention is: the preparation method of the oligosaprobic orange zinc sulfide-based fluorescent material of a kind of high brightness.
In the present invention, Fluorescence Grade zinc sulphide is mixed with dopant ion, fusing assistant, load in double layer aluminium oxide or quartz crucible, fire 2-3 hour, be cooled to room temperature, then screen for 1150-1200 DEG C, washing, dry for standby.Cooled material is mixed with dopant ion, load in aluminum oxide or quartz crucible and carry out double sintering, fire 2-3 hour for 600-800 DEG C, be cooled to room temperature, finally the material after burning is screened, namely washing, oven dry obtain finished product, and described zinc sulphide and the weight ratio of dopant ion are 100: 0.004:0.02:0.01:0.01.The weight ratio of zinc sulphide and fusing assistant is 100:0.06:0.2.
Dopant ion in the present invention is copper, manganese, selenium, cadmium; The compound of the copper of dopant ion is cupric chloride, cupric bromide, copper sulfate; The compound of zinc is zinc oxide, zinc selenide; The compound of manganese is Manganous chloride tetrahydrate, manganous nitrate, Manganese dibromide; Selenium compound is zinc selenide, cadmium selenide, and the compound of cadmium is Cadmium Sulfide.
Fusing assistant in the present invention be muriate as one or more in sodium-chlor, magnesium chloride, ammonium chloride etc., or bromide is as one or more in Sodium Bromide, brometo de amonio, magnesium bromide etc.
The present invention adopts the halogenide only adding nontoxic or low toxicity in the feed if muriate, bromide etc. are as fusing assistant; load in double layer aluminium oxide or quartz crucible; carry out two-step sintering, do not add dithiocarbonic anhydride or hydrogen sulfide but in whole experimentation, only add sulphur as atmosphere protection.The method adopts muriate as one or more in sodium-chlor, magnesium chloride, ammonium chloride etc., or bromide is if one or more in Sodium Bromide, brometo de amonio, magnesium bromide etc. are as fusing assistant, utilize halogenide can dissolve a small amount of zinc sulphide and the zinc oxide producing a small amount of hydrogen sulfide to eliminate wherein and employing have the halogenide of reductibility to eliminate the SO4 in zinc sulphide
2-deng, the zinc chloride simultaneously produced, zinc bromide can promote the crystallization of zinc sulphide.Surface coating uses tin dioxide nanometer material, uses the organic compound material of tin, is prepared by hydrothermal method, and tin dioxide nanometer material uses hydrochloric acid adjustment pH value weakly acidic pH.
the invention has the advantages that
thiscompared with prior art, non-environmental-pollution, manufacturing processed is simple, and easily mass-produced, made fluorescent material, not only for vacuum fluorescence numeral method, also shows for negative ray colour TV pipe in the present invention.
Compared with prior art, the long wave that can affect electroluminescent spectrum moves in the present invention, launches orange red luminescence, is widely used in alternating current-direct current electroluminescence device, makes work exchange voltage be down to safety range under 36V simultaneously.
Embodiment
Embodiment 1
Take 100 grams of ZnS respectively, 6 grams of NaCl, 20 grams of MgCl
2for fusing assistant 0.6 gram of CuSO4.5H
2o, 15ml50%Mn(NO
3)
2, 0.01 gram of ZnSe, 0.01 gram of CdS; Add respectively in watch-glass, finally add 125ml deionized water, put into the oven dry of 120 DEG C, baking oven after stirring, put into double-deck quartz crucible after then the material after oven dry being taken out grinding evenly 1150 DEG C of insulations 2.5 hours, then take out and be at room temperature cooled to room temperature.
Then the material after sintering is poured in ball milling device and add deionized water and carry out wet ball grinding 2 hours.The oven dry of 120 DEG C, baking oven is put into after material deionized water being washed to neutrality after ball milling.Second batch is carried out in material taking-up after drying, adds 2 grams of ZnO, after grinding evenly, add 10ml0.01mol/LCuBr
2solution, 18ml50%Mn(NO
3)
250ml deionized water, then the oven dry of 120 DEG C, baking oven is put into after stirring, load in quartz crucible after drying and be incubated 2.5 hours at 750 DEG C, then take out cooling, after cooling, carry out carrying out washing treatment, first by boiled washed with de-ionized water one time, then soak with acetic acid, then extremely neutral by boiled washed with de-ionized water, finally join caustic dip (volatile salt; 400g, the deionized water 2500ml of boiling, hydrogen peroxide; 600ml, ammoniacal liquor; 1900ml), till being washed till the not aobvious blueness of solution, leaving standstill and pour out alkali lye, then by washed with de-ionized water to neutral, then dry; Surface coating uses tin dioxide nanometer material, uses the organic compound material of tin, is prepared by hydrothermal method, and tin dioxide nanometer material uses hydrochloric acid adjustment pH value weakly acidic pH, and luminosity reaches 80cd/m
2.
Embodiment 2
Take 400 grams of ZnS respectively, 24 grams of NaCl, 80 grams of MgCl
2for fusing assistant 1.6 grams of CuSO4.5H2O, 40 grams of MnCl
2, 4 grams of ZnSe, 4 grams of CdS; Add respectively in watch-glass, finally add 125ml deionized water, put into the oven dry of 120 DEG C, baking oven after stirring, put into double-deck quartz crucible after then the material after oven dry being taken out grinding evenly 1150 DEG C of insulations 2.5 hours, then take out and be at room temperature cooled to room temperature.Then the material after sintering is poured in ball milling device and add deionized water and carry out wet ball grinding 2 hours.The oven dry of 120 DEG C, baking oven is put into after material deionized water being washed to neutrality after ball milling.
Second batch is carried out in material taking-up after drying, adds 8 grams of ZnO, after grinding evenly, add 1.5 grams of CuBr
2, 72ml50%Mn(NO
3)
280ml deionized water, then the oven dry of 120 DEG C, baking oven is put into after stirring, load in quartz crucible after drying and be incubated 2.5 hours at 750 DEG C, then take out cooling, after cooling, carry out carrying out washing treatment, first by boiled washed with de-ionized water one time, then soak with acetic acid, then extremely neutral by boiled washed with de-ionized water, finally join caustic dip (volatile salt; 400g, the deionized water 2500ml of boiling, hydrogen peroxide; 600ml, ammoniacal liquor; 1900ml), till being washed till the not aobvious blueness of solution, leaving standstill and pour out alkali lye, then by washed with de-ionized water to neutral, then dry; Surface coating uses tin dioxide nanometer material, uses the organic compound material of tin, is prepared by hydrothermal method, and tin dioxide nanometer material uses hydrochloric acid adjustment pH value weakly acidic pH, and luminosity reaches 100cd/m
2.
Embodiment 3
Take 800 grams of ZnS respectively, 48 grams of NaCl, 160 grams of MgCl
2for fusing assistant 3.2 grams of CuSO4.5H2O, 80 grams of MnCl
2, 0.08 gram of ZnSe, 0.08 gram of CdS; Add respectively in watch-glass, finally add 125ml deionized water, put into the oven dry of 120 DEG C, baking oven after stirring, put into double-deck quartz crucible after then the material after oven dry being taken out grinding evenly 1150 DEG C of insulations 2.5 hours, then take out and be at room temperature cooled to room temperature.
Then the material after sintering is poured in ball milling device and add deionized water and carry out wet ball grinding 2 hours.The oven dry of 120 DEG C, baking oven is put into after material deionized water being washed to neutrality after ball milling.Second batch is carried out in material taking-up after drying, adds 16 grams of ZnO, after grinding evenly, add 2.0 grams of CuCl
2, 144ml50%Mn(NO
3)
2200ml deionized water, then the oven dry of 120 DEG C, baking oven is put into after stirring, load in quartz crucible after drying and be incubated 2.5 hours at 750 DEG C, then take out cooling, after cooling, carry out carrying out washing treatment, first by boiled washed with de-ionized water one time, then soak with acetic acid, then extremely neutral by boiled washed with de-ionized water, finally join caustic dip (volatile salt; 400g, the deionized water 2500ml of boiling, hydrogen peroxide; 600ml, ammoniacal liquor; 1900ml), till being washed till the not aobvious blueness of solution, leaving standstill and pour out alkali lye, then by washed with de-ionized water to neutral, then dry.Surface coating uses tin dioxide nanometer material, uses the organic compound material of tin, is prepared by hydrothermal method, and tin dioxide nanometer material uses hydrochloric acid adjustment pH value weakly acidic pH, and luminosity reaches 120cd/m
2.
Embodiment 4
Take 1000 grams of ZnS respectively, 60 grams of NaCl, 200 grams of MgCl
2for fusing assistant, 8.0 grams of CuCl
2, 60 grams of MnCl
2, 0.1 gram of ZnSe, 0.1 gram of CdS; Add respectively in watch-glass, finally add 125ml deionized water, put into the oven dry of 120 DEG C, baking oven after stirring, put into double-deck quartz crucible after then the material after oven dry being taken out grinding evenly 1150 DEG C of insulations 2.5 hours, then take out and be at room temperature cooled to room temperature.
Then the material after sintering is poured in ball milling device and add deionized water and carry out wet ball grinding 2 hours.The oven dry of 120 DEG C, baking oven is put into after material deionized water being washed to neutrality after ball milling.Second batch is carried out in material taking-up after drying, adds 20 grams of ZnO, after grinding evenly, add 3.8 grams of CuBr
2, 180ml50%Mn(NO
3)
2300ml deionized water, then the oven dry of 120 DEG C, baking oven is put into after stirring, load in quartz crucible after drying and be incubated 2.5 hours at 750 DEG C, then take out cooling, after cooling, carry out carrying out washing treatment, first by boiled washed with de-ionized water one time, then soak with acetic acid, then extremely neutral by boiled washed with de-ionized water, finally join caustic dip (volatile salt; 400g, the deionized water 2500ml of boiling, hydrogen peroxide; 600ml, ammoniacal liquor; 1900ml), till being washed till the not aobvious blueness of solution, leaving standstill and pour out alkali lye, then by washed with de-ionized water to neutral, then dry.Surface coating uses tin dioxide nanometer material, uses the organic compound material of tin, is prepared by hydrothermal method, and tin dioxide nanometer material uses hydrochloric acid adjustment pH value weakly acidic pH, and luminosity reaches 160cd/m
2.
Embodiment 5
Take 2000 grams of ZnS respectively, 120 grams of NaCl, 400 grams of MgCl
2for fusing assistant, 16 grams of CuBr
2, 120 grams of MnCl
2, 0.2 gram of ZnSe, 0.2 gram of CdS; Add respectively in watch-glass, finally add 125ml deionized water, put into the oven dry of 120 DEG C, baking oven after stirring, put into double-deck quartz crucible after then the material after oven dry being taken out grinding evenly 1150 DEG C of insulations 2.5 hours, then take out and be at room temperature cooled to room temperature.
Then the material after sintering is poured in ball milling device and add deionized water and carry out wet ball grinding 2 hours.The oven dry of 120 DEG C, baking oven is put into after material deionized water being washed to neutrality after ball milling.
Second batch is carried out in material taking-up after drying, adds 40 grams of ZnO, after grinding evenly, add 7.5 grams of CuBr
2, 180 grams of MnCl
2600ml deionized water, then the oven dry of 120 DEG C, baking oven is put into after stirring, load in quartz crucible after drying and be incubated 2.5 hours at 750 DEG C, then take out cooling, after cooling, carry out carrying out washing treatment, first by boiled washed with de-ionized water one time, then soak with acetic acid, then extremely neutral by boiled washed with de-ionized water, finally join caustic dip (volatile salt; 400g, the deionized water 2500ml of boiling, hydrogen peroxide; 600ml, ammoniacal liquor; 1900ml), till being washed till the not aobvious blueness of solution, leaving standstill and pour out alkali lye, then by washed with de-ionized water to neutral, then dry.Surface coating uses tin dioxide nanometer material, uses the organic compound material of tin, is prepared by hydrothermal method, and tin dioxide nanometer material uses hydrochloric acid adjustment pH value weakly acidic pH, and luminosity reaches 140cd/m
2.
Claims (8)
1. the preparation method of the orange red zinc sulfide-based fluorescent material of low-voltage high-brightness, it is characterized in that: Fluorescence Grade zinc sulphide doping dominant activator mn ion, auxiliary activator, fusing assistant are mixed, load in double layer aluminium oxide or quartz crucible, fire 2-3 hour for 1150-1200 DEG C, then at room temperature naturally cooling, then screen, washing, oven dry, Surface coating; Surface coating uses tin dioxide nanometer material, and use hydrochloric acid adjustment pH value weakly acidic pH, it launches orange red luminescence under voltage of alternating current 36V.
2. the preparation method of the orange red zinc sulfide-based fluorescent material of a kind of low-voltage high-brightness according to claim 1, it is characterized in that: cooled material is mixed with dopant ion, load in aluminum oxide or quartz crucible and carry out double sintering, fire 2-3 hour for 600-800 DEG C, be cooled to room temperature, finally screened by the material after burning, namely washing, oven dry obtain finished product.
3. the preparation method of the orange red zinc sulfide-based fluorescent material of a kind of low-voltage high-brightness according to claim 1, is characterized in that: described dopant ion is copper, manganese, selenium, cadmium; Tin dioxide nanometer material uses stanniferous acidic solution, utilizes hydrothermal method to prepare, and mixes, dries with Fluorescence Grade zinc sulphide matrix fluorescent material.
4. the preparation method of the orange red zinc sulfide-based fluorescent material of a kind of low-voltage high-brightness according to claim 1, it is characterized in that: described fusing assistant be muriate as one or more in sodium-chlor, magnesium chloride, ammonium chloride etc. or bromide, as one or more in Sodium Bromide, magnesium bromide, brometo de amonio etc.
5. the preparation method of the orange red zinc sulfide-based fluorescent material of a kind of low-voltage high-brightness according to claim 2, is characterized in that: the compound of the copper of described dopant ion is cupric chloride, cupric bromide, copper sulfate; The compound of zinc is zinc oxide, zinc selenide; The compound of manganese is Manganous chloride tetrahydrate, manganous nitrate, Manganese dibromide; Selenium compound is zinc selenide, cadmium selenide, and the compound of cadmium is Cadmium Sulfide.
6. the preparation method of the orange red zinc sulfide-based fluorescent material of a kind of low-voltage high-brightness according to claim 1, is characterized in that: described washing methods is for first to wash, and then pickling, then be washed to neutrality, subsequently alkali cleaning, is finally washed to neutrality.
7. the preparation method of the orange red zinc sulfide-based fluorescent material of a kind of low-voltage high-brightness according to claim 1, is characterized in that: described alkali lye is volatile salt, deionized water, hydrogen peroxide, the mixing solutions of ammoniacal liquor.
8. the preparation method of the orange red zinc sulfide-based fluorescent material of a kind of low-voltage high-brightness according to claim 1, is characterized in that: tin dioxide nanometer material uses hydrochloric acid adjustment pH value weakly acidic pH, and emmission spectrum is 600nm.
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Application publication date: 20151223 |