CN1451713A - High-brightness long persistence luminescent material composition and preparing method thereof - Google Patents
High-brightness long persistence luminescent material composition and preparing method thereof Download PDFInfo
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- CN1451713A CN1451713A CN 02117237 CN02117237A CN1451713A CN 1451713 A CN1451713 A CN 1451713A CN 02117237 CN02117237 CN 02117237 CN 02117237 A CN02117237 A CN 02117237A CN 1451713 A CN1451713 A CN 1451713A
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- luminescent material
- ammonium chloride
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Abstract
A high-brightness long afterglow luminescent composition has a chemical formula: MO, Al2O3:EU, N, L. The EU2O3 is used as activator, the Dy, Nd, or Gd as sensitizer, and the Al2O3, SrCO3, CaCO3, or BaCO3 as matrix. Its preparing process includes dissolving ammonium chloride or strontium chloride in deionized water, mixing with above-said materials, baking and calcining under the action of flux. Its advantages are high initial brightness and durable luminescence (12 hr).
Description
The present invention relates to a kind of composition and preparation technology thereof of high-brightness luminous material, relate to europium EU specifically
2O
3Rare-earth ion activated, dysprosium Dy
2O
3And gadolinium Gd
2O
3Neodymium Nd
2O
3Composition and preparation technology as the sensitizing agent alkaline earth aluminate persistent luminescent material.
Long after glow luminous material is through sunlight, after light or other light source irradiation, has the accumulation of energy performance, can be luminous for a long time at night or dark place, general effective light can reach more than 6 hours, can circulate and repeat to hold the notion of light and luminous material " effectively twilight sunset ", refer under given conditions in the document,, the apparent time of fluorized marking only gives an example to show explanation more.For instrument, some document adopts following define method, and fluorescent material is painted font No. 6, after ultraviolet ray excited once (10) minute close lamp, in the apparent time of 0.6 meter distance, is called " effectively twilight sunset " time.
Existing phosphor mostly is the sulfide type compound, for example: this sulfide luminescent material of Zns Cu (green light) or ZnCds:Cu (jaundice light) weak point time of persistence 30 minutes 1 hour, and unstable properties, sunlight resistance is poor, work-ing life is short, and preparation technology requires height, the production cost height, because above-mentioned drawback is restricted its application region.
Nineteen nineties, people have developed a kind of aluminate long after glow luminous material, about more existing reports of europkium-activated metal aluminate luminescent material and patent documentation, general preparation method is to be raw material with the oxide compound of aluminium strontium europium or salt that can the above-mentioned oxide compound of corresponding generation after heating: as oxyhydroxide, carbonate etc.The ratio range weighing of each essence component grinds to form fine powder in these compound light-emitting materials chemistries being formed again, uniform mixing, and calcination is at N in 1300 degree-1500 degree high temperature
2+ H
2Gas oxygen in the reduction promptly.This europkium-activated alkali earth metal aluminate long after glow luminous material xln has higher brightness and time of persistence, but because sintering temperature is too high, or add excessive boric acid and reduced sintering temperature, but luminescent material xln hardness is equivalent to jewel in Mohs 6-7 level; This agglomerate is difficult to fragmentation, even if behind the pulverizing and jevigating, it is bigger also to cause powder brightness to reduce.Simultaneously, be N owing to what adopt
2+ H
2Gas mixture makes the security of operation when producing bad, and the equipment difficulty increases, because the too high requirement to heating member of sintering temperature is also higher, productive expense increases again, and cost of manufacture is higher, can not satisfy actual needs.
The objective of the invention is to overcome the not enough technology of improving of prior art, on the proportioning of rare earth, reconfigure, reduce cost, a kind of more high brightness overlength afterglow luminescent material composition is provided.
Another object of the present invention provides that a kind of preparation method is easy, and operability is safe and reliable, the long after glow luminous material method that cost is low.
In order to achieve the above object, the present invention realizes in the following manner.
Chemical constitution formula of the present invention is
MO、Al
2O
3：EU、N、L
Wherein M is Sr or Ca, and one or more of Mg, N are Dy, Nd, Gd one or more, L is an ammonium chloride, strontium chloride.
Preparation technology of the present invention takes following method: raw material adopts corresponding oxide compound or at high temperature changes into compound into oxide compound, i.e. Al
2O
3, SrCO
3, MgCO
3BaCO
3, Srcl and ammonium chloride.Rare earth oxide is EU
2O
3, Dy
2O
3, Gd
2O
3Its consumption is a usage quantity of determining above-mentioned oxide compound or compound according to the ratio of each essence set of dispense in the chemical constitution formula, and its making step is: with rare earth oxide EU
2O
3, Dy
2O
3, Gd
2O
3Putting into container by the portion rate weighing grinds after 20-30 minute and Al
2O
3, SrCO
3, MgCO
3Mix and add an amount of boric acid 1-5% in the hope of reducing sintering temperature, then with strontium oxide, ammonium chloride adds to pour into behind the deionized water dissolving and stirs into pasty state in the said mixture, put into drying baker 120 degree oven dry took out in 20 minutes, batch mixing packed into to go in the corundum crucible in the High Temperature Furnaces Heating Apparatus with carbon granules (AR) cause reducing atmosphere in 1250 ℃ of insulations, the 400 ℃ of taking-ups of after this lowering the temperature naturally in 3-5 hour, promptly get the luminescent material xln, this xln is bulk, and easy pulverizing is ground, owing to adopt the carbon granules atmosphere sintering, sintering and reduction are finished in same operation, and operational safety, cost is low, has very high brightness and steady persistence by long after glow luminous material manufacturing process of the present invention, the china institute of metrology test, use the D65 light source, illuminance is 10001X, excites 10 minutes, can reach 13900 (mcd/m during original intensity 5s
2) 10 hours be 9.6 (mcd/m
2) with existing aluminate luminescent material contrast, see that its brightness exceeds 50%, behind natural light or light-illuminating, can continue luminous more than 12 hours at the dark place.
This long after glow luminous material can mix resin, directly applies in paint, printing ink and the plastics on the ornament or sign class that forms, and becomes light emitting display body through natural light or light-illuminating.As: clock and watch, knob, traffic indication board, doorplate, power switch, artwork, the fire-fighting emergency escape system is debated knowledge etc.
The present invention is further described by the following examples:
Embodiment 1. gets Al
2O
385g, SrCO
398g, CaCO
38.5g, EU
2O
32.5g, Dy
2O
34.8g, Gd
2O
31.2g, H
3BO
322g, Srcl13g, ammonium chloride 16g press weighing with EU
2O
3, Dy
2O
3Gd
2O
3Put into mortar and ground 20 minutes, again with Al
2O
3, SrCO
3, CaCO
3Ground and mixed, rare earth oxide that will grind and aluminium then, strontium, the compound of calcium, the mix grinding time is 1 hour, get strontium chloride 13g, ammonium chloride 16g, use the 50ML deionized water dissolving, pour into then in the above-mentioned compound and stir into pasty state, insert 120 ℃ of oven dry in the drying baker, the raw material of said mixture is put into corundum crucible imbed carbon granule, raw material is not contacted with airborne oxygen, thereby cause a kind of reducing atmosphere, will install the raw material crucible and put into 1250 ℃ of calcination 3-5 of High Temperature Furnaces Heating Apparatus hours, naturally cooling take out below 400 ℃ the bulk xln of yellow-green colour luminescent material, one is 200 orders to grind screening by required fineness, and its original intensity can reach 13900 (mcd/m
2) effectively fluorescent lifetime can reach more than 12 hours.
Embodiment 2
Get Al
2O
365g, SrCO
396g, MgCO
315g, BaCO
325g, ground and mixed were inserted in the High Temperature Furnaces Heating Apparatus 1200 ℃ in 1 hour and are taken out porphyrize after calcination 1.5-2 hour, claimed EU
2O
32.2g, Dy
2O
33.6g, Nd
2O
3, 3.6g, grind and mixed in the said mixture in 20 minutes, mix grinding took out more than 3 hours, with ammonium chloride 15g 48mL deionized water dissolving, being mixed into pasty state with above-mentioned raw materials puts into the oven dry of 120 ℃ of drying bakers and took out in 20 minutes and put into corundum crucible and imbed carbon granule at 1200-1250 ℃, in the High Temperature Furnaces Heating Apparatus calcination 3-5 hour, naturally cooling is below 400 ℃, crucible is taken out cooling back screen granularity with 200 eye mesh screens promptly to obtain color be blue high-brightness long persistence luminescent material from stove, original intensity can reach 6500 (mcd/m
2) effectively after-glow light can reach more than 20 hours.
Claims (4)
1, a kind of high-brightness long persistence luminescent material, composition is characterized in that the chemical expression formula is:
MO、Al
2O
3：EU、N、L。
Wherein M be one or more N of SrC, CaO, BaO, MgO be Dy.Nd.Gd one or more, C is ammonium chloride, strontium chloride.
2, described by claim 1, its composition is than being Al
2O
385g, SrCO
398g, CaCO
38.5g, EU
2O
32.5g, Dy
2O
34.8g, Gd
2O
31.2g, H
3BO
322g, Srcl13g, ammonium chloride 16g, its composition proportioning is a yellow-green light.
3, described by claim 1, its composition is Al
2O
365g, SrCO
396g, MgCO
315g, BaCO
325g, ammonium chloride 15g, its composition proportioning is a blue light.
4, a kind of preparation technology based on claim 1,2,3 described high-brightness long persistence luminescent material compositions.
It is characterized in that may further comprise the steps
(1), rare-earth activated dose of Eu sensitizing agent be that Dy.Nd.ad puts into mortar and ground 20 minutes, puts into compound mixing 1-2 hour of Al, Ca, Mg, Ba.
(2) with strontium chloride, ammonium chloride deionized water dissolving, the material that own step (1) mixes stirs into pasty state and puts into 120 ℃ of oven dry of drying baker 20 minutes, takes out.
(3) will dry good powder, imbed carbon granule 1250 temperature calcinations 3-5 hour in reducing atmosphere in the corundum crucible of packing into.Take out and promptly get the high-brightness long persistence luminescent material xln, this xln is bulk, easily pulverizes and grinds.By required fineness, screening.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02117237 CN1451713A (en) | 2002-04-18 | 2002-04-18 | High-brightness long persistence luminescent material composition and preparing method thereof |
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|---|---|---|---|
| CN 02117237 CN1451713A (en) | 2002-04-18 | 2002-04-18 | High-brightness long persistence luminescent material composition and preparing method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN1451713A true CN1451713A (en) | 2003-10-29 |
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ID=29221096
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|---|---|---|---|
| CN 02117237 Pending CN1451713A (en) | 2002-04-18 | 2002-04-18 | High-brightness long persistence luminescent material composition and preparing method thereof |
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|---|---|
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102911663A (en) * | 2012-09-29 | 2013-02-06 | 浙江工业大学 | White light phosphor powder using calcium carbonate as only substrate and preparation method thereof |
| CN103612449A (en) * | 2013-11-15 | 2014-03-05 | 英利能源（中国）有限公司 | Insulating luminescent material, solar battery back plate comprising insulating luminescent material, and solar battery component |
| CN108690607A (en) * | 2017-11-02 | 2018-10-23 | 王小琴 | A kind of signboard |
-
2002
- 2002-04-18 CN CN 02117237 patent/CN1451713A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102911663A (en) * | 2012-09-29 | 2013-02-06 | 浙江工业大学 | White light phosphor powder using calcium carbonate as only substrate and preparation method thereof |
| CN102911663B (en) * | 2012-09-29 | 2014-09-10 | 浙江工业大学 | White light phosphor powder using calcium carbonate as only substrate and preparation method thereof |
| CN103612449A (en) * | 2013-11-15 | 2014-03-05 | 英利能源（中国）有限公司 | Insulating luminescent material, solar battery back plate comprising insulating luminescent material, and solar battery component |
| CN108690607A (en) * | 2017-11-02 | 2018-10-23 | 王小琴 | A kind of signboard |
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