CN103666465A - Nitride red luminous material with long afterglow and preparation method thereof - Google Patents

Nitride red luminous material with long afterglow and preparation method thereof Download PDF

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CN103666465A
CN103666465A CN201310658485.9A CN201310658485A CN103666465A CN 103666465 A CN103666465 A CN 103666465A CN 201310658485 A CN201310658485 A CN 201310658485A CN 103666465 A CN103666465 A CN 103666465A
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luminous material
roasting
nitride red
raw material
insulation
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黄得财
周有福
许文涛
向明
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Fujian Institute of Research on the Structure of Matter of CAS
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Abstract

The invention discloses a nitride red luminous material with long afterglow and a preparation method thereof. The material has a chemical formula of M<2-x-y>Si5N8:xEu,yRe, wherein in the formula, M is one or more elements selected from Sr, Ca, and Ba, x is more than or equal to 0.005 and less than or equal to 0.15, y is more than or equal to 0.005 and less than or equal to 0.15, and Re represents at least one element selected from the following elements: Tm, Dy, Pr, Nd, Sm, Gd, and Lu. The material comprises at least two rare earth elements. The preparation method obtains a red luminous material with long afterglow, which has the advantages of good chroma, high brightness, and long afterglow time, has the advantages of simple technology, available raw materials, and low cost, and obtains a nitride red luminous material with long afterglow.

Description

Nitride red long after glow luminous material and preparation thereof
Technical field
The present invention relates to rare earth luminescent material technical field, be specifically related to a kind of nitride red long after glow luminous material and preparation method.
Background technology
Rare earth long-afterglow luminescent material is a kind of novel energy-saving environment-friendly material, and it can absorb after the energy of sunlight or light, portion of energy is stored, and then with the form of visible ray, discharge slowly.This characteristic can be widely used in the fields such as illumination, indication and decoration, expands to gradually again in recent years the high-tech areas such as information storage, radiation detection and imaging demonstration.
Traditional long-afterglow material is mainly zinc sulphide (ZnS:Cu) and alkaline earth sulfide (CaS:Bi, Ca, SrS:Bi) etc.Though it is bright-coloured that rare-earth activated long persistence luminous sulfide material has body colour, under the low light level, absorption rate is fast, advantages such as glow color is various, but this class material exists obvious shortcoming are as low in luminosity, fluorescent lifetime is short, poor chemical stability, the easy shortcoming such as deliquescence.Subsequently, the long after glow luminous material that Eu activates comes out successively, and the sixties in 20th century, the researchist of Japan has found SrAl 2o 4: Eu 2+steady persistence phenomenon; The mid-90 in 20th century, scientific worker has developed the New type of S rAl that performance is significantly increased 2o 4: Eu 2+, Dy 3+green glow long-afterglow material.Compare with sulfide material, it is high that aluminate long afterglow materials has luminous efficiency, and time of persistence is long, stable chemical nature, and oxidation-resistance and temperature quenching characteristic are good, no radioactivity pollute, production technique is simple, and low cost and other advantages is developing rapidly in recent ten years.The main shortcoming of aluminate long afterglow materials is that glow color is dull, and emmission spectrum mainly concentrates within the scope of 440～520nm, meets water unstable, and conventional coating processes to improve its water tolerance.
Rare earth ion doped alkaline earth aluminate green and blue long afterflow fluorescent material enter the application stage, red long-afterglow phosphor cannot meet the demand of application always, is mainly because the indexs such as luminosity and time of persistence and yellow-green colour and blue long afterflow fluorescent material exist larger gap.Chinese patent 200910026093.4 and 201210597523.X have reported red long afterglow luminous material Y 2o 2s:Eu 3+, Ti 4+, Mg 2+, its emission wavelength is positioned at 625nm left and right, and can reach 3.5 hours time of persistence, but easily volatilize elemental sulfur in its building-up process, simultaneously poor chemical stability, easily deliquescence.Chinese patent 201210227650.0 has been reported a kind of nitride red long persistence luminescent powder, and its chemical stability is good, luminous efficiency is high, time of persistence is long, but adopts nitride raw material and glove box to mix, and exists raw materials cost high, the deficiencies such as complex process.As realizing one of crucial color of long after glow luminous material red, green, blue scheme of colo(u)r, the research of red long afterglow luminous material is another research emphasis after green and blue twilight sunset material.
Summary of the invention
The object of the invention is to provide a kind of nitride red long after glow luminous material technology of preparing, the raw materials cost of this long after glow luminous material is low, technique is simple, luminous efficiency is high, materialization good stability, within the scope of 300-550nm, can effectively excite, and emission wavelength is between 550-700nm.
The luminescent material that the nitride of take is matrix, the chemical structural formula of described luminescent material is:
M 2-x-ysi 5n 8: xEu, yRe, M is selected from one or more elements of Sr, Ca, Ba, 0.005≤x≤0.15,0.005≤y≤0.15, Re is selected from least one in Tm, Dy, Pr, Nd, Sm, Gd, Lu element.
Another technical problem of the present invention is to provide a kind of preparation method of carbohydrate as reductive agent synthesizing nitride red long afterglow luminous material of usining.Object of the present invention is achieved through the following technical solutions:
The preparation method of nitride luminescent material of the present invention comprises the steps:
(1), according to the chemical constitution of material, by stoichiometric ratio, take M oxide compound or carbonate, Si 3n 4, Eu 2o 3for raw material, the mol ratio of the oxide compound of carbohydrate add-on and metal M or carbonate add-on is 1:(5-7); Add alcohol as grinding medium, in mortar, grind 30-60min, raw material is mixed;
(2) by the step of raw material roasting in inertia or reducing atmosphere; Described reducing gas is the gas mixture of nitrogen and hydrogen, and its volume ratio is (100:0)～(80:20); Roasting first stage rises to 500-800 ℃, makes the complete charing of reductive agent; Roasting second stage rises to 1400-1600 ℃ of insulation 4-8h.Cooling rate with 5 ℃/min～8 ℃/min is cooled to after 250 ℃ afterwards, cools to room temperature with the furnace.
(3) product after roasting is carried out levigate, washing, dry step.
In abovementioned steps (1), described carbohydrate is glucose or sucrose.
In abovementioned steps (1), described M oxide compound or carbonate are BaO, CaO, SrO, BaCO 3caCO 3srCO 3wherein one or more.
The present invention has following features:
The present invention adopt high temperature solid phase synthesis to using carbohydrate as reductive agent, to have prepared series of crystallization degree good, pure phase, the uniform nitride long after glow luminous material of size distribution.Fig. 1 has shown wherein Sr 1.93si 5n 8: 0.02Eu 2+, 0.05Tm 3+the XRD diffracting spectrum of red long afterglow luminous material; Fig. 2 has shown excitation spectrum and the emmission spectrum of this nitride luminescent material, it has very wide excitation band and emission band, excitation spectrum is within the scope of 300～550nm, the strongest excitation peak is positioned near 398nm, at blue light 465nm near zone, have very strong excitation peak, thus this nitride long after glow luminous material can fine coupling LED blue light, UV-light chip.The emission wavelength of this luminescent material is within the scope of 550～700nm, and its emission peak is near 598nm, and luminous intensity is high, and color developing is good.
The invention provides a kind of preparation method of take the nitride red long after glow luminous material that carbohydrate is reductive agent, synthetic target product desired raw material price is low, be easy to obtain and stable in the air, required equipment is simple, the complicated procedures of forming of having avoided glove box to mix.Use carbohydrate as reductive agent, to avoid being mixed with in the ubiquitous product of carbon powder reducing agent the problem of residual carbon dust, sintetics has the good ﹑ good stability of luminous efficiency, brightness advantages of higher simultaneously.
Accompanying drawing explanation
Sr in Fig. 1 example 3 of the present invention 1.93si 5n 8: 0.02Eu 2+, 0.05Tm 3+the XRD diffracting spectrum of red long afterglow luminous material.
Sr in Fig. 2 example 3 of the present invention 1.93si 5n 8: 0.02Eu 2+, 0.05Tm 3+excitation spectrum (the λ of red long afterglow luminous material em=598nm) and emmission spectrum (λ ex=400nm).
Embodiment
Example 1
Press chemical formula Sr 1.99si 5n 8: 0.005Eu, the stoichiometric of 0.005Tm, accurately takes SrCO 3(99.9%), Si 3n 4(99.9%), Eu 2o 3(99.99%), Tm 2o 3(99.99%) raw material, the add-on of dextrose anhydrous and the mol ratio of Strontium carbonate powder are 1:6.
In agate mortar, add appropriate alcohol as grinding medium the above-mentioned raw material weighing up, grind 30～60min raw material is mixed, afterwards, put into 80 ℃ of dry 4h of loft drier, then pack in plumbago crucible, put into high temperature process furnances and heat, heat-up rate with 8 ℃/min rises to 600～700 ℃, insulation 2.5h, then with the heat-up rate of 5 ℃/min, rise to 1500～1600 ℃, insulation 5～6h, cooling rate with 5～10 ℃/min is cooled to 250 ℃ afterwards, cools to room temperature with the furnace.After product after roasting is levigate, the chlorohydric acid pickling that is 1-20wt% by concentration, deionization washing, 5-8 time repeatedly, obtain nitride red long after glow luminous material after being dried.
Example 2
Press chemical formula Sr 1.97si 5n 8: 0.01Eu, the stoichiometric of 0.02Tm, accurately takes SrCO 3(99.9%), Si 3n 4(99.9%), Eu 2o 3(99.99%), Tm 2o 3(99.99%) raw material, the add-on of dextrose anhydrous and the mol ratio of Strontium carbonate powder are 1:6.
Batch mixing process is consistent with example 1 with step.Sample is put into tube furnace, with the heat-up rate of 8 ℃/min, rises to 600～700 ℃, insulation 2.5h, heat-up rate with 5 ℃/min rises to 1500～1600 ℃ again, insulation 5～6h, the cooling rate with 5～10 ℃/min is cooled to 250 ℃ afterwards, cools to room temperature with the furnace.After product after roasting is levigate, the chlorohydric acid pickling that is 1-20wt% by concentration, deionization washing, 5-8 time repeatedly, obtain nitride red long after glow luminous material after being dried.
Example 3
Press chemical formula Sr 1.93si 5n 8: 0.02Eu, the stoichiometric of 0.05Tm, accurately takes SrCO 3(99.9%), Si 3n 4(99.9%), Eu 2o 3(99.99%), Tm 2o 3(99.99%) raw material, the add-on of dextrose anhydrous and the mol ratio of Strontium carbonate powder are 1:6.
Batch mixing process is consistent with example 1 with step.Sample is put into tube furnace, with the heat-up rate of 8 ℃/min, rises to 600～700 ℃, insulation 2.5h, heat-up rate with 5 ℃/min rises to 1500～1600 ℃ again, insulation 5～6h, the cooling rate with 5～10 ℃/min is cooled to 250 ℃ afterwards, cools to room temperature with the furnace.After product after roasting is levigate, the chlorohydric acid pickling that is 1-20wt% by concentration, deionization washing, 5-8 time repeatedly, obtain nitride red long after glow luminous material after being dried.
Example 4
Press chemical formula Sr 1.93si 5n 8: 0.02Eu, the stoichiometric of 0.05Dy, accurately takes SrCO 3(99.9%), Si 3n 4(99.9%), Eu 2o 3(99.99%), Dy 2o 3(99.99%) raw material, the add-on of dextrose anhydrous and the mol ratio of Strontium carbonate powder are 1:6.
Batch mixing process is consistent with example 1 with step.Sample is put into tube furnace, with the heat-up rate of 8 ℃/min, rises to 600～700 ℃, insulation 2.5h, heat-up rate with 5 ℃/min rises to 1500～1600 ℃ again, insulation 5～6h, the cooling rate with 5～10 ℃/min is cooled to 250 ℃ afterwards, cools to room temperature with the furnace.After product after roasting is levigate, the chlorohydric acid pickling that is 1-20wt% by concentration, deionization washing, 5-8 time repeatedly, obtain nitride red long after glow luminous material after being dried.
Example 5
Press chemical formula Sr 1.93si 5n 8: 0.05Eu, the stoichiometric of 0.02Dy, accurately takes SrCO 3(99.9%), Si 3n 4(99.9%), Eu 2o 3(99.99%), Dy 2o 3(99.99%) raw material, the add-on of dextrose anhydrous and the mol ratio of Strontium carbonate powder are 1:6.
Batch mixing process is consistent with example 1 with step.Sample is put into tube furnace, with the heat-up rate of 8 ℃/min, rises to 600～700 ℃, insulation 2.5h, heat-up rate with 5 ℃/min rises to 1500～1600 ℃ again, insulation 5～6h, the cooling rate with 5～10 ℃/min is cooled to 250 ℃ afterwards, cools to room temperature with the furnace.After product after roasting is levigate, the chlorohydric acid pickling that is 1-20wt% by concentration, deionization washing, 5-8 time repeatedly, obtain nitride red long after glow luminous material after being dried.
Example 6
Press chemical formula Ca 1.93si 5n 8: 0.02Eu, the stoichiometric of 0.05Tm, accurately takes CaCO 3(99.9%), Si 3n 4(99.9%), Eu 2o 3(99.99%), Tm 2o 3(99.99%) raw material, the add-on of dextrose anhydrous and the mol ratio of Strontium carbonate powder are 1:6.
Batch mixing process is consistent with example 1 with step.Sample is put into tube furnace, with the heat-up rate of 8 ℃/min, rises to 600～700 ℃, insulation 2.5h, heat-up rate with 5 ℃/min rises to 1500～1600 ℃ again, insulation 5～6h, the cooling rate with 5～10 ℃/min is cooled to 250 ℃ afterwards, cools to room temperature with the furnace.After product after roasting is levigate, the chlorohydric acid pickling that is 1-20wt% by concentration, deionization washing, 5-8 time repeatedly, obtain nitride red long after glow luminous material after being dried.
Example 7
Press chemical formula Ca 1.9si 5n 8: 0.05Eu, the stoichiometric of 0.05Tm, accurately takes CaCO 3(99.9%), Si 3n 4(99.9%), Eu 2o 3(99.99%), Tm 2o 3(99.99%) raw material, the add-on of dextrose anhydrous and the mol ratio of Strontium carbonate powder are 1:6.
Batch mixing process is consistent with example 1 with step.Sample is put into tube furnace, with the heat-up rate of 8 ℃/min, rises to 600～700 ℃, insulation 2.5h, heat-up rate with 5 ℃/min rises to 1500～1600 ℃ again, insulation 5～6h, the cooling rate with 5～10 ℃/min is cooled to 250 ℃ afterwards, cools to room temperature with the furnace.After product after roasting is levigate, the chlorohydric acid pickling that is 1-20wt% by concentration, deionization washing, 5-8 time repeatedly, obtain nitride red long after glow luminous material after being dried.
Example 8
Press chemical formula Ca 1.93si 5n 8: 0.05Eu, the stoichiometric of 0.02Tm, accurately takes CaCO 3(99.9%), Si 3n 4(99.9%), Eu 2o 3(99.99%), Tm 2o 3(99.99%) raw material, the add-on of dextrose anhydrous and the mol ratio of Strontium carbonate powder are 1:6.
Batch mixing process is consistent with example 1 with step.Sample is put into tube furnace, with the heat-up rate of 8 ℃/min, rises to 600～700 ℃, insulation 2.5h, heat-up rate with 5 ℃/min rises to 1500～1600 ℃ again, insulation 5～6h, the cooling rate with 5～10 ℃/min is cooled to 250 ℃ afterwards, cools to room temperature with the furnace.After product after roasting is levigate, the chlorohydric acid pickling that is 1-20wt% by concentration, deionization washing, 5-8 time repeatedly, obtain nitride red long after glow luminous material after being dried.
Example 9
Press chemical formula Ca 1.96si 5n 8: 0.02Eu, the stoichiometric of 0.02Dy, accurately takes CaCO 3(99.9%), Si 3n 4(99.9%), Eu 2o 3(99.99%), Dy 2o 3(99.99%) raw material, the add-on of dextrose anhydrous and the mol ratio of Strontium carbonate powder are 1:6.
Batch mixing process is consistent with example 1 with step.Sample is put into tube furnace, with the heat-up rate of 8 ℃/min, rises to 600～700 ℃, insulation 2.5h, heat-up rate with 5 ℃/min rises to 1500～1600 ℃ again, insulation 5～6h, the cooling rate with 5～10 ℃/min is cooled to 250 ℃ afterwards, cools to room temperature with the furnace.After product after roasting is levigate, the chlorohydric acid pickling that is 1-20wt% by concentration, deionization washing, 5-8 time repeatedly, obtain nitride red long after glow luminous material after being dried.
Example 10
Press chemical formula Ca 1.94si 5n 8: 0.02Eu, 0.02Dy, the stoichiometric of 0.02Tm, accurately takes CaCO 3(99.9%), Si 3n 4(99.9%), Eu 2o 3(99.99%), Tm 2o 3(99.99%), Dy 2o 3(99.99%) raw material, the add-on of dextrose anhydrous and the mol ratio of Strontium carbonate powder are 1:6.
Batch mixing process is consistent with example 1 with step.Sample is put into tube furnace, with the heat-up rate of 8 ℃/min, rises to 600～700 ℃, insulation 2.5h, heat-up rate with 5 ℃/min rises to 1500～1600 ℃ again, insulation 5～6h, the cooling rate with 5～10 ℃/min is cooled to 250 ℃ afterwards, cools to room temperature with the furnace.After product after roasting is levigate, the chlorohydric acid pickling that is 1-20wt% by concentration, deionization washing, 5-8 time repeatedly, obtain nitride red long after glow luminous material after being dried.
Example 11
Press chemical formula Ba 1.93si 5n 8: 0.02Eu, the stoichiometric of 0.05Tm, accurately takes BaCO 3(99.9%), Si 3n 4(99.9%), Eu 2o 3(99.99%), Tm 2o 3(99.99%) raw material, the add-on of dextrose anhydrous and the mol ratio of Strontium carbonate powder are 1:6.
Batch mixing process is consistent with example 1 with step.Sample is put into tube furnace, with the heat-up rate of 8 ℃/min, rises to 600～700 ℃, insulation 2.5h, heat-up rate with 5 ℃/min rises to 1500～1600 ℃ again, insulation 5～6h, the cooling rate with 5～10 ℃/min is cooled to 250 ℃ afterwards, cools to room temperature with the furnace.After product after roasting is levigate, the chlorohydric acid pickling that is 1-20wt% by concentration, deionization washing, 5-8 time repeatedly, obtain nitride red long after glow luminous material after being dried.
Example 12
Press chemical formula Ba 1.93si 5n 8: 0.02Eu, the stoichiometric of 0.05Dy, accurately takes BaCO 3(99.9%), Si 3n 4(99.9%), Eu 2o 3(99.99%), Dy 2o 3(99.99%) raw material, the add-on of dextrose anhydrous and the mol ratio of Strontium carbonate powder are 1:6.
Batch mixing process is consistent with example 1 with step.Sample is put into tube furnace, with the heat-up rate of 8 ℃/min, rises to 600～700 ℃, insulation 2.5h, heat-up rate with 5 ℃/min rises to 1500～1600 ℃ again, insulation 5～6h, the cooling rate with 5～10 ℃/min is cooled to 250 ℃ afterwards, cools to room temperature with the furnace.After product after roasting is levigate, the chlorohydric acid pickling that is 1-20wt% by concentration, deionization washing, 5-8 time repeatedly, obtain nitride red long after glow luminous material after being dried.

Claims (4)

1. nitride red long after glow luminous material, chemical structural formula is: M 2-x-ysi 5n 8: xEu, yRe, M is selected from one or more elements of Sr, Ca, Ba, 0.005≤x≤0.15,0.005≤y≤0.15, Re is selected from least one in Tm, Dy, Pr, Nd, Sm, Gd, Lu element.
2. the preparation method of nitride red long after glow luminous material, comprises the steps:
(1) by the oxide compound of raw material M or carbonate, Si 3n 4, Eu 2o 3with the mixed uniformly step of reductive agent; Described raw material is pressed M 2-x-ysi 5n 8: xEu, the stoichiometric ratio of yRe takes; The oxide compound of described reductive agent add-on and M or the mol ratio of carbonate add-on are 1:(5-8); M is selected from one or more elements of Sr, Ca, Ba, 0.005≤x≤0.15, and 0.005≤y≤0.15, Re is selected from least one in Tm, Dy, Pr, Nd, Sm, Gd, Lu element;
(2) by the step of raw material roasting in inertia or reducing atmosphere; Described reducing gas is the gas mixture of nitrogen and hydrogen, and its volume ratio is (100:0)～(80:20); Roasting first stage rises to 500-800 ℃, makes the complete charing of reductive agent; Roasting second stage rises to 1400-1600 ℃ of insulation 4-8h.
3. method according to claim 2, is characterized in that: described reductive agent is glucose or sucrose.
4. method according to claim 2, is characterized in that: described M oxide compound or carbonate are BaO, CaO, SrO, BaCO 3caCO 3srCO 3wherein one or more.
CN201310658485.9A 2013-12-09 2013-12-09 Nitride red luminous material with long afterglow and preparation method thereof Pending CN103666465A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104726095A (en) * 2015-02-03 2015-06-24 五邑大学 Low-energy-consumption method for preparing nitride red fluorescent powder under normal atmosphere
CN105238395A (en) * 2015-09-24 2016-01-13 华南农业大学 Silicon-based nitride red fluorescent powder, and normal pressure preparation method and applications thereof
CN105385014A (en) * 2015-12-11 2016-03-09 华南农业大学 Light conversion agricultural film, and making method and application thereof

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JP2009074077A (en) * 2007-08-31 2009-04-09 Mitsubishi Chemicals Corp Phosphor, composition containing this phosphor, luminescent device, lighting system, and image display
CN101831295A (en) * 2010-04-07 2010-09-15 江苏博睿光电有限公司 Silica-based nitride red fluorescent powder and preparation method thereof
CN102766454A (en) * 2012-06-30 2012-11-07 江苏博睿光电有限公司 Nitride red long-afterglow fluorescent powder and preparation method thereof
CN103305213A (en) * 2013-05-28 2013-09-18 中国科学院福建物质结构研究所 Method for preparing nitride phosphor powder

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009074077A (en) * 2007-08-31 2009-04-09 Mitsubishi Chemicals Corp Phosphor, composition containing this phosphor, luminescent device, lighting system, and image display
CN101831295A (en) * 2010-04-07 2010-09-15 江苏博睿光电有限公司 Silica-based nitride red fluorescent powder and preparation method thereof
CN102766454A (en) * 2012-06-30 2012-11-07 江苏博睿光电有限公司 Nitride red long-afterglow fluorescent powder and preparation method thereof
CN103305213A (en) * 2013-05-28 2013-09-18 中国科学院福建物质结构研究所 Method for preparing nitride phosphor powder

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104726095A (en) * 2015-02-03 2015-06-24 五邑大学 Low-energy-consumption method for preparing nitride red fluorescent powder under normal atmosphere
CN104726095B (en) * 2015-02-03 2017-04-12 五邑大学 Low-energy-consumption method for preparing nitride red fluorescent powder under normal atmosphere
CN105238395A (en) * 2015-09-24 2016-01-13 华南农业大学 Silicon-based nitride red fluorescent powder, and normal pressure preparation method and applications thereof
CN105385014A (en) * 2015-12-11 2016-03-09 华南农业大学 Light conversion agricultural film, and making method and application thereof

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