CN1513944A - Field emitting white luminuous material containing rare earth element sulfide and its manufacturing method - Google Patents
Field emitting white luminuous material containing rare earth element sulfide and its manufacturing method Download PDFInfo
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- CN1513944A CN1513944A CNA021605483A CN02160548A CN1513944A CN 1513944 A CN1513944 A CN 1513944A CN A021605483 A CNA021605483 A CN A021605483A CN 02160548 A CN02160548 A CN 02160548A CN 1513944 A CN1513944 A CN 1513944A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
A field-emitting luminescent material (size 3-20 micron) containing RE sulfide for emitting white light contains M2OS2, where M is chosen from Y, Gd, La and Lu, the component A chosen from Eu and Tb, and component B chosen from Ga, Pr, Ge, Sc, Ce, In, Tl, Er and Mn. Its preparing process is also disclosed. Its light wavelength is 450-610 nm.
Description
Technical field
The present invention relates to field emission light-emitting material and manufacture method thereof in the shiner Neo-Confucianism, more particularly, the present invention relates to a kind of field emission white luminescent material and manufacture method thereof that comprises rare earth element sulfide.
Background technology
The employed luminescent powder of existing field emission light-emitting (FED) device is the special-purpose luminescent material of cathodoluminescence (CRT) device, it is the luminescent material based on zinc sulphide and rare earth oxide or sulfide, these luminescent materials all have bigger deficiency to the FED device on the burning property of Yan Zaikang, life-span, luminous efficiency, when especially working under strong excitaton source state.In the Chinese patent application 00102920,96193775 this all there is relevant introduction.
Summary of the invention
The purpose of this invention is to provide a kind of rare earth material that uses through specific technical process white luminous powdered material of produced rare earth element sulfide and manufacture method thereof, the granularity of described powdered material is in the scope of 3-20 micron, radiative wavelength is 450-610nm, and it has the good characteristics of luminescence in the application of FED device.
The invention provides a kind of field emission white luminescent material that comprises rare earth element sulfide, in the gross weight of material, it comprises (a) 90-99% general formula is M
2OS
2In the oxysulfide one or more, wherein M represents yttrium, gadolinium, lanthanum or lutetium, and O represents oxygen, and S represents sulphur; (b) 0.01-5% element europium and terbium; (c) one or more in 0.02-5% element gallium, praseodymium, germanium, scandium, cerium, indium, thallium, erbium or the manganese.Component in above-mentioned materials (b) is element europium and element terbium, and their weight ratio is 1: 25-25: 1.
Material of the present invention also comprises and accounts for component (a) and (b) and (c) fusing assistant of the 0-40 weight % of total amount, and described fusing assistant is selected from H
3BO
3, Na
2CO
3, BaF
3, (NH
4)
2HPO
4, LiPO
3, Li
2CO
3, BaCO
3, K
3PO
4, MnF and Na
3PO
4In one or more.
The granularity of material of the present invention is the 3-20 micron.
The present invention also provides a kind of method of emission white luminescent material of making, it comprises yttrium, gadolinium, the oxide compound of lanthanum or lutetium or in the inorganic salt one or more, the oxide compound of europium and terbium or inorganic salt and gallium, praseodymium, germanium, scandium, cerium, indium, thallium, the oxide compound of erbium or manganese or in the inorganic salt one or more mix in certain proportion, the high-purity sulphur that adds the 10-50% that accounts for the lucium gross weight, mixing the back grinds evenly, under 1000-1300 ℃ temperature in air sintering 2-5 hour, make the field emission white luminescent material that comprises rare earth element sulfide.
The present invention also provides another kind of and makes as a method of launching white luminescent material, it comprises yttrium, gadolinium, the oxide compound of lanthanum or lutetium or in the inorganic salt one or more, the oxide compound of europium and terbium or inorganic salt and gallium, praseodymium, germanium, scandium, cerium, indium, thallium, the oxide compound of erbium or manganese or in the inorganic salt one or more mix in certain proportion, after grinding evenly, be added in the aqueous nitric acid that concentration is 10-40 weight %, in the time of 50-90 ℃, make above-mentioned each material dissolution become water white solution, be added to again in the oxalic acid aqueous solution that concentration is 5-50 weight %, same under 50-90 ℃ temperature, make raw material be precipitated as the oxalate white precipitate of rare earth element, with this throw out in 800-1200 ℃ air sintering 1-5 hour, form the mixture of rare earth oxide, the high-purity sulphur that adds the 10-50% that accounts for rare earth oxide mixture total weight amount therein, mixing the back grinds evenly, under 1000-1300 ℃ temperature in air sintering 2-5 hour, comprise the field emission white luminescent material of rare earth element sulfide.
In above-mentioned manufacture method, described inorganic salt comprise halogenide or nitrate.In addition, in aforesaid method, before 1000-1300 ℃ temperature sintering, when adding high-purity sulphur, can also add fusing assistant.
Except above-mentioned steps, method of the present invention comprises that also the material to gained carries out the surface-coating processing, its process is to add surface-coating treatment solution and distilled water in the luminescent material of gained, luminescent material wherein: the surface-coating treatment solution: the weight ratio of distilled water is 1: (0.01-1): (2-10), after the stirring, regulate the pH value to 5-8, oven dry.In this surface-coating was handled, described surface-coating treatment solution was K
2SiO
3, Na
2SiO
3Or Al
2(SO
4)
3In one or more solution in distilled water, the weight ratio of described compound or mixture and distilled water is 1: 20-1: 3.
Purpose of the present invention specifically is achieved through the following channels.
In the gross weight of material, the field emission white luminescent material that comprises rare earth element sulfide involved in the present invention comprises following three kinds of components:
(a) the 90-99% general formula is M
2OS
2In the oxysulfide one or more, wherein M represents yttrium (Y), gadolinium (Gd), lanthanum (La) or lutetium (Lu), and O represents oxygen, and S represents sulphur.This component (a) can be Y specifically
2OS
2, La
2OS
2, Y
2OS
2+ Lu
2OS
2, Gd
2OS
2+ La
2OS
2And Y
2OS
2+ Gd
2OS
2+ Lu
2OS
2Deng.By following manufacture method of the present invention as can be known, with the oxide compound of the rare earth element of M representative or inorganic salt obtain component (a) behind high temperature sintering in sulphur and oxygen atmosphere oxysulfide, its chemical equation is MP+S+ air=M
2OS
2, wherein M represents above-mentioned rare earth element, and MP represents the oxide compound or the inorganic salt (comprising halogenide, nitrate etc.) of above-mentioned rare earth element, and O represents oxygen, and S represents sulphur.When component (a) is two or more oxysulfide, to the ratio between each oxysulfide and without particular limitation, as long as their total amount is in above-mentioned scope.
(b) 0.01-5% element europium (Eu) and element terbium (Tb), i.e. Eu+Tb.By following manufacture method of the present invention as can be known, because through high temperature sintering, the material that the present invention makes forms crystal to a certain degree, detect through X-light ray diffraction approach, discovery europium and terbium are filled out in the lattice of component (a) oxysulfide with the form of element.In the present invention, ratio between element europium and the element terbium also there is certain restriction, the weight ratio that is them is 1: 25-25: 1, wherein the ratio of Eu for a long time emmission spectrum move to long wave, the ratio of Tb emmission spectrum for a long time moves to shortwave, owing to use europium and terbium simultaneously, the emission on the scene of prepared material issues comes from light.
(c) one or more in 0.02-5% element gallium (Ga), praseodymium (Pr), germanium (Ge), scandium (Sc), cerium (Ce), indium (In), thallium (Tl), erbium (Er) or the manganese (Mn), this component can be Ga+Pr, Ge+In, Ga+Er+Mn, Pr+Ge+Ce+In, Tl+Er and Pr+Ge+Tl+Mn etc. specifically.By following manufacture method of the present invention as can be known, because through high temperature sintering, the material that the present invention makes forms crystal to a certain degree, detect through X-light ray diffraction approach, one or more forms with element in gallium, praseodymium, germanium, scandium, cerium, indium, thallium, erbium or the manganese of finding are filled out in the lattice of component (a) oxysulfide, when component (c) is two or more elements, to the ratio between each element and without particular limitation, as long as their total amount is in above-mentioned scope.
Except said components (a)-(c), material of the present invention can also comprise and accounts for component (a) and (b) and (c) fusing assistant of the 0-40 weight % of total amount, and described fusing assistant is selected from H
3BO
3, Na
2CO
3, BaF
3, (NH
4)
2HPO
4, LiPO
3, Li
2CO
3, BaCO
3, K
3PO
4, MnF and Na
3PO
4In one or more.That is to say that this component is an optional components, this component specifically can be Na
2CO
3, H
3BO
3+ (NH
4)
2HPO
4And Li
2CO
3+ K
3PO
4+ Na
3PO
4Deng.When this component is two or more compounds, to the ratio between each compound and without particular limitation, as long as their total amount is in above-mentioned scope.
The material that the present invention makes generally is pulverous form, and its granularity is generally the 3-20 micron, is preferably the 3-8 micron.
The present invention also provides the manufacture method of above-mentioned materials, with regard to manufacture method, generally is divided into dry method and wet method.
Dry method at first is described.(be yttrium with matrix earlier, gadolinium, the oxide compound of lanthanum or lutetium or in the inorganic salt one or more), activator (being the oxide compound or the inorganic salt of europium and terbium) and coactivator (are gallium, praseodymium, germanium, scandium, cerium, indium, thallium, the oxide compound of erbium or manganese or in the inorganic salt one or more) mix in certain proportion, in above-mentioned matrix, inorganic salt described in activator and the coactivator comprise halogenide or nitrate etc., described ratio be make in the obtained material each components contents within the limits prescribed, in general, the ratio of each raw material of adding is identical with the ratio of each respective components in the products therefrom.Then, adding high-purity sulphur and the optional fusing assistant of the 10-50% account for the lucium gross weight, mix the back and grind evenly, is that purity is 99.9% or above sulphur at this used high-purity sulphur.Then, under 1000-1300 ℃ temperature in air sintering 2-5 hour, promptly in sulphur and oxygen atmosphere through high temperature sintering, make the field emission white luminescent material that comprises rare earth element sulfide.
Next illustrates wet method.(be yttrium with matrix earlier, gadolinium, the oxide compound of lanthanum or lutetium or in the inorganic salt one or more), activator (being the oxide compound or the inorganic salt of europium and terbium) and coactivator (are gallium, praseodymium, germanium, scandium, cerium, indium, thallium, the oxide compound of erbium or manganese or in the inorganic salt one or more) mix in certain proportion, grind evenly, in above-mentioned matrix, inorganic salt described in activator and the coactivator comprise halogenide or nitrate etc., described ratio be make in the obtained material each components contents within the limits prescribed, in general, the ratio of each raw material of adding is identical with the ratio of each respective components in the products therefrom.Then, said mixture is added in the aqueous nitric acid that concentration is 10-40 weight %, make above-mentioned each material dissolution become water white solution in the time of 50-90 ℃, the consumption to aqueous nitric acid in this process is also without particular limitation, just can as long as mixture is dissolved fully.Then, the solution of gained is added in the oxalic acid aqueous solution that concentration is 5-50 weight %, same under 50-90 ℃ temperature, make raw material be precipitated as the oxalate white precipitate of rare earth element, consumption to oxalic acid aqueous solution in this process is also without particular limitation, just can as long as solution is precipitated fully.To precipitate through clear water and clean, in 120 ℃ of oven dry.Then, with this throw out in 800-1200 ℃ air sintering 1-5 hour, form the mixture of rare earth oxide.The mixture of rare earth oxide also can be obtained like this, promptly directly with the abundant ground and mixed of matrix/activator/coactivator evenly after, directly in the air of 800-1200 degree sintering 1-5 hour.Then, adding high-purity sulphur and the optional fusing assistant of the 10-50% account for rare earth oxide mixture total weight amount therein, mix the back and grind evenly, is that purity is 99.9% or above sulphur at this used high-purity sulphur.Then, under 1000-1300 ℃ temperature in air sintering 2-5 hour, promptly in sulphur and oxygen atmosphere through high temperature sintering, make the field emission white luminescent material that comprises rare earth element sulfide.
In addition, better be the above-mentioned material that makes to be carried out surface-coating handle, its objective is in order to improve anti-the burning property of gained material.The material that obtains is above cleaned 3 times with distilled water, add surface-coating treatment solution and distilled water, luminescent material wherein: the surface-coating treatment solution: the weight ratio of distilled water is 1: (0.01-1): (2-10), after the stirring of above-mentioned substance thorough mixing, use as 10% ammoniacal liquor is regulated the pH value to 5-8, pour out after the excessive solution 120 ℃ of oven dry.In above-mentioned treating processes, described surface-coating treatment solution is K
2SiO
3, Na
2SiO
3Or Al
2(SO
4)
3In one or more solution in distilled water, the weight ratio of described compound or mixture and distilled water is 1: 20-1: 3.
Compared with the prior art, the present invention has following advantage.At first, the granularity of the powdered material that the present invention makes is in the scope of 3-20 micron, and radiative wavelength is 450-610nm, promptly sends white light, and it has the good characteristics of luminescence in the application of FED device.Secondly, use material of the present invention, especially the FED device that makes of the material after surface-coating is handled has extraordinary anti-burning property, and the brightness decay of promptly putting after 100 hours is at most 5%, and the brightness decay of FED device after putting 100 hours made from common CRT material is up to 20-30%.Moreover, owing to anti-the burning property of the FED device made from material of the present invention is good, so this device lifetime is long, the luminous efficiency foot.In addition, material of the present invention also can be used for the FED illuminating device.
Embodiment
In conjunction with following embodiment the present invention is described in further detail now, but what should understand is that the present invention is not limited to these certain embodiments.
In the following embodiments, it is synthetic that used feed composition is the laboratory, and the model of used spectrograph is SPR-920D when detecting.
Embodiment 1
Get Y
2O
397 grams, Eu
2O
30.091 gram, Tb
4O
70.063 gram and Ga
2O
30.94 gram.With the abundant ground and mixed of above-mentioned raw materials evenly after, be added in the aqueous nitric acid that 300 ml concns are 10 weight %, be heated to 80 ℃ temperature, be dissolved into water white solution, be added to again in the oxalic acid aqueous solution that 200 ml concns are 10 weight %, temperature at 70 ℃ is reacted, the reaction back generates the oxalate white precipitate of rare earth element, throw out is after clear water cleans, in 120 ℃ of oven dry 10 hours, dried rare earth element oxalate precipitation thing sintering 1 hour in 1100 ℃ air forms the mixture of rare earth oxide.Adding 15 gram purity are 99.9% sulphur in said mixture, after abundant ground and mixed is even, in the quartz crucible with cover of packing into, place 1000 ℃ of high-temperature electric resistance furnace sintering 5 hours, form the rare-earth sulfide luminescent material.
After with distilled water above-mentioned materials being cleaned 3 times, add surface-coating treatment solution and distilled water, the surface-coating treatment solution is 5 gram Na
2SiO
3Be dissolved in the solution that obtains in 100 ml distilled waters, luminescent material wherein: surface-coating treatment solution: distillation water=1: 1: 5 (weight ratio), above-mentioned substance is mixed, fully stirred 1 hour, use 10% ammoniacal liquor that its pH value is adjusted to 7, dry at 120 degree after pouring out excessive solution.
The material of gained contains column element: Y, O, Eu, Tb, Ga and S down through spectroscopic analysis.The material of analyzing gained through X-ray diffraction comprises Y
2OS
2, element Eu, element T b and element Ga.
Send the white light of high brightness under the above-mentioned materials emission on the scene, use its luminous wave band of spectrometer measurement in the scope of 450-610nm.
Embodiment 2-6
Repeat the process of embodiment 1, the different raw materials that are to use different compositions and amount the results are shown in the following table 1.
Table 1
| Embodiment | Raw material | Product | |||||||||||
| Matrix | Activator | Coactivator | Fusing assistant | Component (a) | Component (b) | Component (c) | Luminous | ||||||
| Form | Consumption, g | Form | Consumption, g | Form | Consumption, g | Form | Consumption, g | Color | Wavelength, nm | ||||
| Embodiment 2 | ??YCl 3 | ??99 | ???Eu 2O 3???+Tb 4O 7 | ??0.1+ ??0.1 | ??GaCl 3+Ge 2O 3 | ??3 | ?- | ?- | ?Y 2OS 2 | ?Eu+Tb | ?Ga+Ge | Brilliant white | ??460- ??600 |
| Embodiment 3 | ??Y 2O 3+La 2O ??3 | ??96 | ???Eu 2O 3???+Tb 4O 7 | ??1+3 | ??Pr 2O 3+Er 2O 3 | ??4 | ?H 3BO 3+ ?Na 2CO 3 | ?10.4 | ?Y 2OS 2+ ?La 2OS 2 | ?Eu+Tb | ?Pr+Er | Brilliant white | ??480- ??520 |
| Embodiment 4 | ??Y(NO 3) 3+G ??d(NO 3) 3 | ??90 | ???Eu(NO 3) 3???+Tb(NO 3???)3 | ??2+3 | ??Tl(NO 3) 3+Ce(N ??O 3) 3+Er(NO 3) 3 | ??5 | ?Li 2CO 3?+K 3PO 4 | ?40 | ?Y 2OS 2+ ?Gd 2OS 2 | ?Eu+Tb | ?Tl+Ce ?+Er | Brilliant white | ??450- ??590 |
| Embodiment 5 | ??LuCl 3 | ??95 | ???EuCl 3+T ???bCl 3 | ??3+2 | ??ScCl 3+InCl 3+M ??nCl 3+GaCl 3 | ??5 | ?- | ?- | ?Lu 2OS 2 | ?Eu+Tb | ?Sc+In ?+Mn+G ?a | Brilliant white | ??500- ??580 |
| Embodiment 6 | ??Y(NO 3) 3+L ??aBr 3 | ??93 | ???Eu(NO 3) 3???+TbBr 3 | ??1+3 | ??Ga(NO 3) 3+CeBr ?? 3 | ??5 | ?Li 2CO 3?+BaCO ? 3+MnF | ?40.8 | ?Y 2OS 2+ ?La 2OS 2 | ?Eu+Tb | ?Ga+Ce | Brilliant white | ??520- ??600 |
Embodiment 7
Get La
2O
398 grams, Eu
2O
31.5 gram, Tb
2O
70.7 gram and Sc
2O
33.5 gram, with the abundant ground and mixed of above-mentioned raw materials evenly after, in said mixture, add 50 gram purity and be 99.9% sulphur, after abundant ground and mixed is even, pack in the quartz crucible with cover, placed 1300 ℃ of high-temperature electric resistance furnace sintering 2 hours, form the rare-earth sulfide luminescent material.
After with distilled water above-mentioned materials being cleaned 3 times, add surface-coating treatment solution and distilled water, the surface-coating treatment solution is 5 gram Na
2SiO
3With 5 gram K
2SiO
3Be dissolved in the solution that obtains in 30 ml distilled waters, luminescent material wherein: surface-coating treatment solution: distillation water=1: 0.01: 10 (weight ratio), above-mentioned substance is mixed, fully stirred 1 hour, use 10% ammoniacal liquor that its pH value is adjusted to 5, dry at 120 degree after pouring out excessive solution.
The material of gained contains column element: La, O, Eu, Tb, Sc and S down through spectroscopic analysis.The material of analyzing gained through X-ray diffraction comprises La
2OS
2, element Eu, element T b and element S c.
Send the white powder red light of high brightness under the above-mentioned materials emission on the scene, use its luminous wave band of spectrometer measurement in the scope of 450-610nm.
Embodiment 8-12
Repeat the process of embodiment 7, the different raw materials that are to use different compositions and amount the results are shown in the following table 2.
Table 2
| Embodiment | Raw material | Product | |||||||||||
| Matrix | Activator | Coactivator | Fusing assistant | Component (a) | Component (b) | Component (c) | Luminous | ||||||
| Form | Consumption, g | Form | Consumption, g | Form | Consumption, g | Form | Consumption, g | ?- | ?- | ?- | Color | Wavelength, nm | |
| Embodiment 8 | ?YCl 3 | ??99 | ??Eu 2O 3??+Tb 4O 7 | ??0.1+ ??0.1 | ??PrC1 3+Er 2O 3 | ??3 | ??- | ?- | ?Y 2OS 2 | ?Eu+Tb | ?Ga+Ge | The brilliant white pink | ??460- ??600 |
| Embodiment 9 | ?Y 2O 3+La 2O ?3 | ??96 | ??Eu 2O 3??+Tb 4O 7 | ??1+3 | ??Ga 2O 3+Tl 2O 3 | ??4 | ?H 3BO 3+ ?Na 2CO 3 | ?10.4 | ?Y 2OS 2+ ?La 2OS 2 | ?Eu+Tb | ?Pr+Er | The brilliant white pink | ??480- ??520 |
| Embodiment 10 | ?Y(NO 3) 3+G ?d(NO 3) 3 | ??90 | ??Eu(NO 3) 3??+Tb(NO 3??) 3 | ??2+3 | ??Tl(NO 3) 3+Ce(N ??O 3) 3+Sc(NO 3) 3 | ??5 | ?Li 2CO 3?+K 3PO 4 | ?40 | ?Y 2OS 2+ ?Gd 2OS 2 | ?Eu+Tb | ?Tl+Ce ?+Er | The brilliant white pink | ??450- ??590 |
| Embodiment 11 | ?LuCl 3 | ??95 | ??EuCl 3+T ??bCl 3 | ??3+2 | ??ScCl 3+InCl 3+M ??nCl 3+GaCl 3 | ??5 | ?- | ?- | ?Lu 2OS 2 | ?Eu+Tb | ?Sc+In ?+Mn+G ?a | The brilliant white pink | ??500- ??580 |
| Embodiment 12 | ?Y(NO 3) 3+L ?aBr 3 | ??93 | ??Eu(NO 3) 3??+TbBr 3 | ??1+3 | ??Ga(NO 3) 3+InBr ?? 3 | ??5 | ?Li 2CO 3?+BaCO ? 3+MnF | ?40.8 | ?Y 2OS 2+ ?La 2OS 2 | ?Eu+Tb | ?Ga+Ce | The brilliant white pink | ??520- ??600 |
After specific embodiments of the present invention had been done above-mentioned detailed description, what it will be appreciated by those skilled in the art that was under the situation that does not depart from spirit and scope of the invention, can make various changes and improvements to it.
Claims (10)
1. white luminescent material is launched in a field that comprises rare earth element sulfide, and in the gross weight of material, it comprises (a) 90-99% general formula is M
2OS
2In the oxysulfide one or more, wherein M represents yttrium, gadolinium, lanthanum or lutetium, and O represents oxygen, and S represents sulphur; (b) 0.01-5% element europium and terbium; (c) one or more in 0.02-5% element gallium, praseodymium, germanium, scandium, cerium, indium, thallium, erbium or the manganese.
2. material as claimed in claim 1, wherein component (b) is element europium and element terbium, their weight ratio is 1: 25-25: 1.
3. material as claimed in claim 1 or 2, it also comprises and accounts for component (a) and (b) and (c) fusing assistant of the 0-40 weight % of total amount, and described fusing assistant is selected from H
3BO
3, Na
2CO
3, BaF
3, (NH
4)
2HPO
4, LiPO
3, Li
2CO
3, BaCO
3, K
3PO
4, MnF and Na
3PO
4In one or more.
4. material as claimed in claim 1 or 2, wherein the granularity of material is the 3-20 micron.
5. make the method for material according to claim 1 for one kind, it comprise with the oxide compound of yttrium, gadolinium, lanthanum or lutetium or in the inorganic salt one or more, the oxide compound of the oxide compound of europium and terbium or inorganic salt and gallium, praseodymium, germanium, scandium, cerium, indium, thallium, erbium or manganese or in the inorganic salt one or more mix in certain proportion, the high-purity sulphur that adds the 10-50% that accounts for the lucium gross weight, mixing the back grinds evenly, under 1000-1300 ℃ temperature in air sintering 2-5 hour, make the field emission white luminescent material that comprises rare earth element sulfide.
6. make the method for material according to claim 1 for one kind, it comprises yttrium, gadolinium, the oxide compound of lanthanum or lutetium or in the inorganic salt one or more, the oxide compound of europium and terbium or inorganic salt and gallium, praseodymium, germanium, scandium, cerium, indium, thallium, the oxide compound of erbium or manganese or in the inorganic salt one or more mix in certain proportion, after grinding evenly, be added in the aqueous nitric acid that concentration is 10-40 weight %, in the time of 50-90 ℃, make above-mentioned each material dissolution become water white solution, be added to again in the oxalic acid aqueous solution that concentration is 5-50 weight %, same under 50-90 ℃ temperature, make raw material be precipitated as the oxalate white precipitate of rare earth element, with this throw out in 800-1200 ℃ air sintering 1-5 hour, form the mixture of rare earth oxide, the high-purity sulphur that adds the 10-50% that accounts for rare earth oxide mixture total weight amount therein, mixing the back grinds evenly, under 1000-1300 ℃ temperature in air sintering 2-5 hour, make the field emission white luminescent material that comprises rare earth element sulfide.
7. as claim 5 or 6 described methods, wherein said inorganic salt comprise halogenide or nitrate.
8. as claim 5 or 6 described methods, wherein before 1000-1300 ℃ temperature sintering, when adding high-purity sulphur, add fusing assistant.
9. as claim 5 or 6 described methods, it comprises that also the material to gained carries out the surface-coating processing, its process is to add surface-coating treatment solution and distilled water in the luminescent material of gained, luminescent material wherein: the surface-coating treatment solution: the weight ratio of distilled water is 1: (0.01-1): (2-10), after the stirring, regulate the pH value to 5-8, oven dry.
10. method as claimed in claim 9, wherein said surface-coating treatment solution is K
2SiO
3, Na
2SiO
3Or Al
2(SO
4)
3In one or more solution in distilled water, the weight ratio of described compound or mixture and distilled water is 1: 20-1: 3.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100368283C (en) * | 2005-11-05 | 2008-02-13 | 大连海事大学 | Method for preparing fine rare earth sulfoxides |
| CN103849399A (en) * | 2012-11-29 | 2014-06-11 | 海洋王照明科技股份有限公司 | Oxysulfide luminescent material and preparation method thereof |
| CN105154061A (en) * | 2015-10-01 | 2015-12-16 | 上海洞舟实业有限公司 | Transparent damp-proof film wrapping method for electroluminescence powder |
| CN105315995A (en) * | 2015-12-03 | 2016-02-10 | 河北利福光电技术有限公司 | Fluxing agent and method for preparing YAG fluorescent powder |
-
2002
- 2002-12-31 CN CNB021605483A patent/CN1255508C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100368283C (en) * | 2005-11-05 | 2008-02-13 | 大连海事大学 | Method for preparing fine rare earth sulfoxides |
| CN103849399A (en) * | 2012-11-29 | 2014-06-11 | 海洋王照明科技股份有限公司 | Oxysulfide luminescent material and preparation method thereof |
| CN103849399B (en) * | 2012-11-29 | 2016-04-20 | 海洋王照明科技股份有限公司 | oxysulfide luminescent material and preparation method thereof |
| CN105154061A (en) * | 2015-10-01 | 2015-12-16 | 上海洞舟实业有限公司 | Transparent damp-proof film wrapping method for electroluminescence powder |
| CN105315995A (en) * | 2015-12-03 | 2016-02-10 | 河北利福光电技术有限公司 | Fluxing agent and method for preparing YAG fluorescent powder |
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| Publication number | Publication date |
|---|---|
| CN1255508C (en) | 2006-05-10 |
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